#------------------------------------------------------------------------------ #$Date: 2022-03-03 21:16:18 +0000 (Thu, 03 Mar 2022) $ #$Revision: 273270 $ #$URL: svn://www.crystallography.net/cod/cif/4/51/93/4519363.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4519363 loop_ _publ_author_name 'D'souza, Luann R.' 'Harmalkar, Nikita N.' 'Harmalkar, Sarvesh S.' 'Tayade, Sakharam B.' 'Dhuri, Sunder N.' _publ_section_title ; Construction of Pyrazine-Appended 1D and 3D Cobalt(II) Succinate Coordination Polymers: Influence of Solvent on Architectures and Applications in Gas Adsorption and NAC Detection. ; _journal_issue 7 _journal_name_full 'ACS omega' _journal_page_first 5698 _journal_page_last 5712 _journal_paper_doi 10.1021/acsomega.1c05216 _journal_volume 7 _journal_year 2022 _chemical_formula_sum 'C4 H12 Co O8' _chemical_formula_weight 247.07 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2017/1 _cell_angle_alpha 90 _cell_angle_beta 99.7410(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.4075(3) _cell_length_b 14.8143(6) _cell_length_c 7.7787(3) _cell_measurement_reflns_used 6370 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 28.24 _cell_measurement_theta_min 2.75 _cell_volume 841.30(6) _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker D8 Quest Eco' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_unetI/netI 0.0212 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 12443 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.272 _diffrn_reflns_theta_min 2.750 _exptl_absorpt_coefficient_mu 2.056 _exptl_absorpt_correction_type none _exptl_crystal_colour pink _exptl_crystal_density_diffrn 1.951 _exptl_crystal_description block _exptl_crystal_F_000 508 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.366 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.062 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 142 _refine_ls_number_reflns 2080 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.0283 _refine_ls_R_factor_gt 0.0225 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+0.4804P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.0596 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1849 _reflns_number_total 2085 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ao1c05216_si_007.cif _cod_data_source_block 06 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 4519363 _shelx_shelxl_version_number 2017/1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; TITL 03crystal_0m_a.res in P2(1)/c 03crystal_0m_a.res created by SHELXL-2017/1 at 01:30:23 on 18-Jul-2019 REM Old TITL 03crystal_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.076, Rweak 0.003, Alpha 0.036, Orientation as input REM Formula found by SHELXT: C4 Co O8 CELL 0.71073 7.4075 14.8143 7.7787 90.000 99.741 90.000 ZERR 12.000 0.0003 0.0006 0.0003 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H CO O UNIT 16 48 4 32 ACTA TEMP 23.000 L.S. 10 BOND $H HTAB LIST 6 FMAP 2 PLAN 20 WGHT 0.026300 0.480400 FVAR 0.69928 CO1 3 0.570622 0.355438 0.812304 11.00000 0.01527 0.01968 = 0.01229 -0.00120 -0.00158 0.00078 C1 1 -0.066062 0.382678 0.053608 11.00000 0.01607 0.01817 = 0.01618 0.00244 -0.00407 0.00137 O1 4 0.633989 0.216906 0.820499 11.00000 0.03658 0.02444 = 0.01575 0.00038 0.00155 0.00796 AFIX 148 H1 2 0.676890 0.204558 0.908533 11.00000 -1.50000 AFIX 0 O2 4 0.767700 0.370616 0.642401 11.00000 0.02206 0.02296 = 0.01769 0.00046 -0.00109 -0.00115 AFIX 148 H2 2 0.762130 0.421719 0.602995 11.00000 -1.50000 AFIX 0 C2 1 0.038436 0.419838 0.223123 11.00000 0.02237 0.02477 = 0.02031 -0.00263 -0.00723 0.00078 AFIX 23 H2A 2 0.122493 0.465957 0.196520 11.00000 -1.20000 H2AB 2 -0.047608 0.448406 0.287159 11.00000 -1.20000 AFIX 0 O4 4 0.383820 0.339867 0.981756 11.00000 0.01461 0.02908 = 0.02227 0.00426 0.00096 0.00057 AFIX 148 H4 2 0.300488 0.353569 0.942117 11.00000 -1.50000 AFIX 0 C4 1 0.266498 0.388239 0.497948 11.00000 0.01694 0.02475 = 0.01297 0.00054 -0.00146 -0.00108 O3 4 0.519784 0.494635 0.799474 11.00000 0.03801 0.02225 = 0.02703 -0.00622 -0.00878 0.00416 AFIX 148 H3 2 0.435204 0.505149 0.720645 11.00000 -1.50000 AFIX 0 C3 1 0.145743 0.349132 0.338492 11.00000 0.02658 0.02369 = 0.01763 -0.00086 -0.00751 -0.00041 AFIX 23 H3A 2 0.221805 0.315860 0.270506 11.00000 -1.20000 H3AB 2 0.060524 0.306792 0.376247 11.00000 -1.20000 AFIX 0 O5 4 0.260019 0.470483 0.529947 11.00000 0.03987 0.02362 = 0.02416 -0.00193 -0.01227 0.00345 H5 2 0.384277 0.288560 1.015941 11.00000 0.05162 O7 4 0.018790 0.367409 -0.069135 11.00000 0.01671 0.04107 = 0.02006 -0.00239 -0.00036 0.00373 H7 2 0.524002 0.532252 0.871316 11.00000 0.07013 O6 4 0.369569 0.332767 0.593828 11.00000 0.02405 0.02400 = 0.01671 -0.00140 -0.00805 0.00237 H6 2 0.673738 0.194684 0.749387 11.00000 0.04637 O8 4 -0.237749 0.371652 0.042287 11.00000 0.01569 0.04145 = 0.01464 -0.00253 -0.00182 -0.00496 H8 2 0.852573 0.366729 0.707774 11.00000 0.02784 HKLF 4 REM 03crystal_0m_a.res in P2(1)/c REM R1 = 0.0225 for 1849 Fo > 4sig(Fo) and 0.0283 for all 2080 data REM 142 parameters refined using 0 restraints END WGHT 0.0263 0.4804 REM Instructions for potential hydrogen bonds EQIV $3 x, -y+1/2, z+1/2 HTAB O1 O2_$3 EQIV $4 -x+1, -y+1, -z+1 HTAB O2 O5_$4 EQIV $5 -x, -y+1, -z+1 HTAB C2 O5_$5 EQIV $6 x, y, z+1 HTAB O4 O7_$6 HTAB O3 O5 HTAB C3 O7_$3 HTAB O4 O6_$3 EQIV $7 -x+1, -y+1, -z+2 HTAB O3 O4_$7 EQIV $8 x+1, -y+1/2, z+1/2 HTAB O1 O8_$8 EQIV $2 x+1, y, z+1 HTAB O2 O7_$2 REM Highest difference peak 0.366, deepest hole -0.315, 1-sigma level 0.062 Q1 1 -0.0062 0.3986 0.1358 11.00000 0.05 0.37 Q2 1 0.2082 0.3665 0.4189 11.00000 0.05 0.36 Q3 1 0.4425 0.3544 0.6441 11.00000 0.05 0.27 Q4 1 0.1406 0.3000 0.3197 11.00000 0.05 0.25 Q5 1 0.3312 0.4576 0.4799 11.00000 0.05 0.25 Q6 1 0.2394 0.3538 0.9720 11.00000 0.05 0.24 Q7 1 -0.2834 0.3474 -0.0342 11.00000 0.05 0.23 Q8 1 -0.2754 0.3715 -0.0471 11.00000 0.05 0.23 Q9 1 -0.0199 0.3909 -0.0292 11.00000 0.05 0.22 Q10 1 0.4346 0.4752 0.8433 11.00000 0.05 0.21 Q11 1 0.0910 0.3866 0.2697 11.00000 0.05 0.20 Q12 1 -0.0099 0.3436 -0.0030 11.00000 0.05 0.19 Q13 1 0.1096 0.3576 -0.0619 11.00000 0.05 0.19 Q14 1 -0.2861 0.3797 0.0904 11.00000 0.05 0.19 Q15 1 0.8163 0.3426 0.5577 11.00000 0.05 0.18 Q16 1 -0.1611 0.3906 0.0482 11.00000 0.05 0.18 Q17 1 0.0372 0.3984 -0.1041 11.00000 0.05 0.18 Q18 1 0.2211 0.4393 0.5590 11.00000 0.05 0.17 Q19 1 0.0820 0.2832 0.0091 11.00000 0.05 0.17 Q20 1 0.1661 0.4523 0.4887 11.00000 0.05 0.17 ; _shelx_res_checksum 53481 _shelx_hkl_file ; -2 0 0 554.04 16.50 -2 0 0 541.35 16.60 -2 0 0 533.45 13.90 2 0 0 539.05 16.20 2 0 0 542.95 16.40 2 0 0 537.45 13.90 3 0 0 355.86 14.20 3 0 0 368.66 11.50 -3 0 0 407.06 15.10 -3 0 0 386.56 15.10 -3 0 0 362.96 11.60 3 0 0 366.26 14.30 -4 0 0 153.48 10.10 -4 0 0 159.18 7.50 -4 0 0 156.38 10.30 4 0 0 172.18 7.70 -5 0 0 1902.31 47.70 -5 0 0 1896.81 52.39 -5 0 0 1771.12 51.89 6 0 0 1554.34 39.40 -6 0 0 1470.75 38.90 -6 0 0 1551.64 48.70 -6 0 0 1536.95 47.60 7 0 0 278.37 12.60 -7 0 0 307.67 18.90 -7 0 0 273.47 18.90 -8 0 0 6.40 4.90 8 0 0 3.30 2.50 -9 0 0 25.30 8.80 -9 0 0 47.60 9.10 -1 -1 0 492.95 13.00 -1 -1 0 479.75 12.40 -1 -1 0 457.05 12.20 -1 1 0 487.65 12.80 1 1 0 484.85 14.00 -1 1 0 479.45 12.90 -2 -1 0 774.22 19.90 -2 -1 0 769.12 21.10 2 -1 0 783.12 17.50 2 -1 0 766.02 21.30 2 -1 0 796.02 21.60 -2 -1 0 808.32 21.90 -2 1 0 760.92 21.30 -2 1 0 766.82 21.70 2 1 0 782.62 21.50 2 1 0 807.02 20.10 2 1 0 736.43 20.70 -2 1 0 775.02 17.50 -3 -1 0 236.68 9.40 3 -1 0 237.88 7.60 -3 -1 0 242.68 11.10 3 -1 0 224.18 10.80 3 -1 0 235.08 10.90 -3 -1 0 217.38 11.00 3 1 0 230.28 11.00 -3 1 0 222.28 10.90 -3 1 0 228.88 11.20 3 1 0 236.38 10.80 3 1 0 231.38 9.20 -3 1 0 232.88 7.60 -4 -1 0 1621.34 42.80 4 -1 0 1617.44 37.30 -4 -1 0 1635.74 45.10 -4 -1 0 1683.83 44.30 -4 1 0 1606.24 37.30 -4 1 0 1619.94 44.60 4 1 0 1654.83 43.00 -4 1 0 1555.84 44.20 -5 -1 0 1293.97 40.00 5 -1 0 1200.08 30.70 -5 -1 0 1223.48 33.70 -5 -1 0 1289.57 39.00 -5 1 0 1265.77 39.40 5 1 0 1257.17 33.80 -5 1 0 1287.97 39.60 -5 1 0 1235.78 30.90 6 -1 0 170.58 8.20 -6 -1 0 180.68 13.60 -6 -1 0 165.28 12.80 -6 1 0 155.48 12.90 -6 1 0 189.18 13.70 6 1 0 164.08 9.70 -6 1 0 164.88 9.20 -7 -1 0 -0.50 3.40 -7 -1 0 4.00 3.00 7 -1 0 3.50 2.80 -7 1 0 4.20 4.50 7 1 0 0.70 2.40 -7 1 0 -0.50 3.80 8 -1 0 30.30 5.50 -8 -1 0 29.90 7.60 -8 1 0 27.90 7.90 8 1 0 30.50 5.10 -9 -1 0 212.78 18.40 -9 -1 0 250.07 21.20 9 1 0 256.87 13.00 -9 1 0 252.27 20.80 -9 1 0 236.58 19.90 0 -2 0 174.18 5.60 -1 -2 0 550.64 15.00 -1 -2 0 550.74 14.00 1 -2 0 575.94 12.40 1 2 0 569.04 15.40 1 2 0 569.04 15.10 -1 2 0 559.24 12.50 1 2 0 537.15 13.90 -1 2 0 579.74 14.80 2 -2 0 6.90 2.00 -2 -2 0 6.40 1.80 -2 -2 0 7.10 1.90 -2 -2 0 11.40 2.60 2 -2 0 7.70 2.10 2 2 0 7.20 1.90 2 2 0 7.90 2.00 -2 2 0 10.10 2.40 2 2 0 10.40 2.50 -2 2 0 8.80 2.50 -3 -2 0 561.44 19.50 -3 -2 0 573.04 20.80 3 -2 0 563.24 19.30 3 -2 0 579.24 12.90 -3 -2 0 567.14 18.70 3 -2 0 535.95 18.60 -3 2 0 559.34 13.00 3 2 0 562.34 17.60 3 2 0 563.64 19.60 -3 2 0 557.14 19.40 -3 2 0 510.45 18.50 -4 -2 0 1680.53 45.70 4 -2 0 1714.43 37.70 -4 -2 0 1696.13 43.60 -4 -2 0 1761.02 47.50 -4 2 0 1727.13 37.80 -4 2 0 1762.02 47.00 4 2 0 1750.12 43.60 -4 2 0 1773.92 47.40 -5 -2 0 537.25 21.70 -5 -2 0 509.45 22.40 5 -2 0 501.95 13.90 -5 2 0 496.15 13.90 -5 2 0 517.85 22.20 5 2 0 505.25 18.70 -5 2 0 503.05 21.90 6 -2 0 11.10 2.20 -6 -2 0 9.70 4.30 -6 -2 0 8.60 3.90 -6 2 0 14.60 2.30 6 2 0 14.60 3.70 -6 2 0 13.50 4.30 -6 2 0 15.20 5.10 -7 -2 0 11.60 5.40 -7 -2 0 6.40 3.80 7 -2 0 8.90 1.90 -7 2 0 9.20 4.50 7 2 0 7.70 3.50 -7 2 0 13.60 5.60 -7 2 0 5.20 2.00 -8 -2 0 7.70 5.20 -8 -2 0 9.20 9.80 -9 -2 0 17.90 7.00 -9 -2 0 14.00 6.70 -9 2 0 13.80 5.90 -9 2 0 13.30 7.40 0 -3 0 6.40 1.40 0 -3 0 5.20 1.40 0 3 0 2.70 1.00 0 3 0 5.60 1.40 0 3 0 4.60 1.50 1 -3 0 0.90 0.90 -1 -3 0 -0.20 1.00 -1 -3 0 2.10 1.30 1 -3 0 1.70 1.20 1 -3 0 0.60 1.10 -1 -3 0 6.50 2.00 1 3 0 2.20 1.10 -1 3 0 2.20 1.20 1 3 0 2.30 1.60 1 3 0 1.20 1.00 -1 3 0 2.20 0.90 -1 3 0 1.90 1.60 -2 -3 0 0.10 1.40 2 -3 0 4.10 1.60 -2 -3 0 0.80 1.30 -2 -3 0 3.20 1.60 2 -3 0 2.00 1.60 -2 3 0 1.70 1.70 2 3 0 1.00 1.60 2 3 0 2.50 1.70 2 3 0 3.20 1.30 -2 3 0 2.80 1.60 -3 -3 0 58.69 5.90 -3 -3 0 76.69 5.90 -3 -3 0 57.99 5.40 3 -3 0 70.69 7.40 3 -3 0 71.99 7.10 -3 3 0 76.29 6.60 3 3 0 53.99 8.90 -3 3 0 62.49 6.00 3 3 0 78.19 6.00 -4 -3 0 942.21 30.60 -4 -3 0 958.70 29.10 -4 3 0 909.71 29.60 -4 3 0 912.61 30.40 4 3 0 926.61 27.90 -5 -3 0 348.77 18.20 -5 -3 0 352.46 17.20 -5 3 0 401.16 18.80 5 3 0 343.57 15.50 -5 3 0 368.56 19.30 -6 -3 0 33.60 7.40 -6 -3 0 33.60 6.50 6 3 0 31.00 5.60 -6 3 0 34.40 7.10 -6 3 0 38.00 7.50 -7 -3 0 14.50 5.70 -7 -3 0 21.30 5.80 -7 3 0 12.10 5.70 -7 3 0 21.00 6.10 7 3 0 8.60 3.80 -8 -3 0 38.30 9.40 -8 -3 0 19.40 6.10 -8 3 0 31.70 9.20 8 3 0 41.80 6.80 -9 -3 0 122.79 14.20 -9 -3 0 136.29 16.10 -9 3 0 112.29 16.10 9 3 0 101.89 9.90 -9 3 0 121.29 17.00 -1 -4 0 34.30 3.70 1 -4 0 40.70 3.40 -1 -4 0 29.90 2.80 1 -4 0 31.60 2.80 -1 -4 0 33.40 3.60 -1 -4 0 32.80 2.80 -1 4 0 29.60 3.50 1 4 0 29.70 2.60 1 4 0 42.50 4.40 -1 4 0 30.00 3.30 -1 4 0 35.00 3.00 -2 -4 0 134.89 6.70 2 -4 0 124.29 4.30 2 -4 0 139.29 7.80 2 4 0 113.99 7.00 -2 4 0 132.79 4.60 -2 4 0 128.49 10.80 -2 4 0 130.69 4.40 2 4 0 142.39 6.50 2 4 0 132.49 8.00 -2 4 0 123.79 7.70 -3 -4 0 50.79 4.90 -3 -4 0 60.79 5.90 3 4 0 54.09 5.60 3 4 0 50.99 9.00 -3 4 0 57.59 5.60 -3 4 0 47.80 5.70 -4 -4 0 6.60 3.10 -4 -4 0 10.50 3.20 -4 4 0 11.60 3.70 -4 4 0 8.50 2.80 4 4 0 13.70 3.80 -5 -4 0 1566.64 48.80 -5 -4 0 1579.54 45.70 -5 4 0 1648.44 47.70 5 4 0 1656.53 45.20 -5 4 0 1602.94 49.20 -6 -4 0 1331.67 44.90 -6 -4 0 1299.47 48.80 -6 4 0 1354.26 45.10 -6 4 0 1350.56 44.10 6 4 0 1281.57 40.00 -7 -4 0 499.05 24.50 -7 -4 0 499.35 26.30 -7 4 0 470.15 25.50 -7 4 0 473.75 25.20 -8 -4 0 122.79 12.90 -8 -4 0 126.59 14.50 -8 4 0 123.29 14.50 -8 4 0 120.19 13.80 8 4 0 126.99 11.10 -9 -4 0 89.49 12.70 -9 -4 0 87.99 14.60 -9 4 0 104.39 15.80 -9 4 0 85.59 13.90 9 4 0 107.19 10.90 0 -5 0 0.50 1.50 0 -5 0 2.00 1.20 0 -5 0 2.40 1.50 0 5 0 1.20 1.60 0 5 0 3.30 1.50 0 5 0 1.70 1.40 1 -5 0 646.14 19.30 -1 -5 0 684.03 19.90 -1 -5 0 687.13 18.10 1 -5 0 663.83 18.20 1 -5 0 658.03 19.20 1 -5 0 736.53 20.10 -1 -5 0 698.73 17.90 1 5 0 666.63 20.90 -1 5 0 659.23 18.40 -1 5 0 685.53 19.40 1 5 0 669.83 19.50 -1 5 0 671.93 19.60 2 -5 0 104.09 6.80 -2 -5 0 101.19 7.30 -2 -5 0 120.09 7.50 -2 -5 0 106.39 6.10 2 -5 0 98.69 4.50 2 -5 0 106.69 6.60 -2 5 0 110.69 7.30 2 5 0 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255.77 16.30 -8 -4 3 255.57 19.00 -8 4 3 229.28 18.70 8 4 -3 222.58 14.80 -7 -4 3 97.79 9.30 -7 -4 3 81.49 11.50 7 4 -3 106.39 10.20 -7 4 3 91.09 12.80 -7 4 3 99.99 11.70 -6 -4 3 3.20 2.00 6 -4 -3 -0.30 1.30 6 -4 -3 -0.20 1.40 -6 -4 3 3.70 3.30 -6 4 3 -3.10 2.50 6 4 -3 -0.80 2.20 -6 4 3 0.60 2.70 -5 -4 3 289.17 12.70 5 -4 -3 280.67 10.40 -5 -4 3 273.17 15.10 5 -4 -3 278.57 10.30 5 4 -3 277.87 15.00 -5 4 3 274.07 16.00 -5 4 3 291.17 16.50 5 4 -3 267.97 12.30 -4 -4 3 706.83 24.10 4 -4 -3 702.03 20.20 -4 -4 3 697.83 20.40 -4 4 3 706.43 25.90 -4 4 3 687.53 25.70 4 4 -3 746.23 25.80 4 4 -3 679.53 20.20 -4 4 3 688.33 19.90 -3 -4 3 889.91 25.80 -3 -4 3 926.31 22.30 3 -4 -3 874.91 25.10 -3 4 3 966.80 32.30 3 4 -3 903.41 28.90 -3 4 3 903.41 29.10 -3 4 3 909.41 28.90 3 4 -3 882.81 25.70 3 4 -3 881.01 22.20 -2 -4 3 330.07 10.90 2 -4 -3 322.37 14.40 2 -4 -3 313.67 12.60 2 4 -3 324.07 14.70 -2 4 3 310.77 14.00 2 4 -3 323.57 11.00 -2 4 3 344.37 14.80 -2 4 3 314.37 12.70 2 4 -3 344.57 9.00 2 4 -3 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13.50 5 3 -9 136.89 11.30 -5 3 9 151.88 14.60 5 3 -9 156.48 10.70 5 3 -9 151.48 16.50 4 -3 -9 120.69 12.70 4 -3 -9 87.09 13.00 4 3 -9 96.79 14.50 4 3 -9 94.69 9.50 -4 3 9 99.79 12.10 4 3 -9 79.99 7.60 3 -3 -9 344.77 19.90 -3 -3 9 318.67 22.30 3 3 -9 342.27 18.20 3 3 -9 336.97 24.40 -3 3 9 321.47 22.30 3 3 -9 314.57 13.60 -2 -3 9 63.39 10.70 2 -3 -9 58.99 8.90 2 3 -9 66.09 9.60 -2 3 9 43.00 10.00 2 3 -9 41.00 9.90 -1 -3 9 1.60 4.40 1 -3 -9 3.80 4.80 1 -3 -9 5.50 4.00 1 3 -9 3.10 4.00 -1 3 9 -4.80 4.80 0 -3 9 128.49 14.80 0 -3 -9 124.39 11.60 0 -3 -9 140.39 15.10 0 3 -9 122.49 13.40 0 3 9 123.79 14.20 -1 -3 -9 48.50 11.10 -1 -3 -9 33.00 7.50 1 -3 9 64.59 12.50 1 3 9 37.40 10.10 -1 3 -9 43.10 9.00 -2 -3 -9 252.17 18.00 -2 -3 -9 299.87 23.10 2 -3 9 298.47 22.40 -2 3 -9 272.67 20.80 2 3 9 322.77 23.70 -3 -3 -9 212.18 20.60 3 -3 9 207.68 18.70 3 3 9 153.78 17.90 -3 3 -9 190.08 18.20 5 -4 -9 -1.40 5.10 5 -4 -9 3.00 4.80 5 -4 -9 3.30 4.90 5 4 -9 -1.60 5.30 4 -4 -9 42.00 9.70 4 -4 -9 42.50 8.90 -4 4 9 37.10 8.40 4 4 -9 46.00 7.20 4 4 -9 30.50 9.60 -3 -4 9 8.90 5.00 3 -4 -9 -0.20 4.30 3 -4 -9 8.70 5.10 3 4 -9 17.40 7.00 -3 4 9 4.90 5.50 3 4 -9 8.90 3.90 2 -4 -9 23.60 7.60 -2 -4 9 20.00 7.50 2 -4 -9 22.00 6.50 2 4 -9 24.70 5.50 -2 4 9 18.00 6.60 2 4 -9 36.80 9.30 1 -4 -9 49.00 8.80 1 -4 -9 62.79 11.40 -1 -4 9 48.30 10.20 -1 4 9 49.30 9.90 1 4 -9 47.80 11.10 1 4 -9 50.79 8.50 0 -4 -9 87.49 12.20 0 -4 -9 90.89 13.70 0 -4 9 94.29 14.20 0 4 9 103.59 15.40 0 4 -9 110.09 12.00 1 -4 9 25.00 7.50 -1 -4 -9 21.00 6.90 -1 -4 -9 16.80 8.00 -1 4 -9 27.00 7.80 1 4 9 28.70 8.10 2 -4 9 9.60 5.80 -2 -4 -9 -2.00 5.10 -2 -4 -9 4.70 6.20 -2 4 -9 8.70 5.90 2 4 9 13.10 7.00 5 -5 -9 5.50 4.90 5 -5 -9 17.60 7.40 5 5 -9 11.60 6.50 -5 5 9 7.90 5.90 4 -5 -9 -3.10 4.50 4 -5 -9 -3.70 6.20 4 5 -9 0.70 5.10 -4 5 9 4.90 4.50 3 -5 -9 16.10 7.10 3 -5 -9 29.70 8.40 -3 5 9 30.30 8.30 3 5 -9 26.20 5.90 3 5 -9 28.20 9.10 -2 -5 9 41.20 9.60 2 -5 -9 36.70 8.30 2 -5 -9 37.70 10.10 -2 5 9 44.80 9.80 2 5 -9 32.00 5.80 2 5 -9 34.40 9.90 -1 -5 9 -0.70 3.50 1 -5 -9 2.80 4.80 1 -5 -9 3.20 5.00 1 5 -9 1.90 3.80 1 5 -9 -7.90 4.60 -1 5 9 -5.00 4.10 0 -5 -9 82.19 11.70 0 -5 -9 82.19 14.10 0 -5 9 70.79 12.60 0 5 -9 63.09 10.30 0 5 -9 73.79 14.00 0 5 9 60.69 12.30 -1 -5 -9 8.70 6.20 1 -5 9 5.50 6.30 -1 -5 -9 4.50 5.90 -1 5 -9 -6.90 4.70 1 5 9 1.90 4.60 -1 5 -9 -5.10 5.50 -2 -5 -9 6.90 6.50 2 -5 9 1.70 5.70 -2 -5 -9 5.80 6.60 2 5 9 1.50 5.00 -2 5 -9 9.80 7.10 5 -6 -9 22.50 7.90 5 -6 -9 58.59 11.00 5 6 -9 33.20 9.60 -5 6 9 33.20 7.90 4 -6 -9 12.10 6.80 4 -6 -9 6.90 4.60 4 6 -9 8.70 6.30 -4 6 9 4.10 4.60 3 -6 -9 46.50 11.00 3 -6 -9 74.49 13.70 3 6 -9 62.99 12.20 3 6 -9 48.60 8.40 -3 6 9 75.09 11.30 2 -6 -9 139.49 14.50 2 -6 -9 133.19 15.80 2 6 -9 155.58 17.20 -2 6 9 171.18 16.50 1 -6 -9 236.08 17.70 1 -6 -9 238.38 20.20 -1 -6 9 217.88 19.40 -1 6 9 218.18 19.10 1 6 -9 234.18 20.50 1 6 -9 232.28 14.80 0 -6 -9 338.07 24.80 0 -6 9 324.87 23.70 0 -6 -9 372.56 26.40 0 6 -9 366.26 20.50 0 6 9 358.76 24.50 0 6 -9 363.36 25.80 -1 -6 -9 27.30 8.30 -1 -6 -9 28.50 8.90 1 -6 9 39.00 9.90 1 6 9 23.50 8.70 -1 6 -9 26.50 10.10 -1 6 -9 32.70 8.10 -2 -6 -9 5.90 6.30 2 -6 9 35.00 9.00 -2 -6 -9 20.50 9.00 -2 6 -9 26.30 9.00 -2 6 -9 13.90 6.60 2 6 9 24.20 8.60 4 -7 -9 162.18 17.20 4 -7 -9 200.48 17.70 -4 7 9 197.78 17.80 4 7 -9 189.98 19.00 3 -7 -9 553.64 31.40 3 -7 -9 553.14 29.30 3 7 -9 547.75 32.00 -3 7 9 504.55 29.00 2 -7 -9 119.19 13.40 2 -7 -9 134.49 15.70 -2 7 9 107.39 15.20 2 7 -9 118.79 17.10 2 7 -9 108.19 14.60 1 -7 -9 27.80 8.40 1 -7 -9 25.00 8.20 1 7 -9 24.60 6.00 1 7 -9 24.40 8.60 -1 7 9 11.30 6.60 0 -7 9 146.39 16.60 0 -7 -9 178.68 17.60 0 -7 -9 143.29 14.50 0 7 9 177.48 18.10 0 7 -9 165.08 17.90 0 7 -9 187.28 13.00 -1 -7 -9 136.09 16.30 1 -7 9 129.69 15.50 -1 -7 -9 164.78 16.20 -1 7 -9 136.89 16.60 1 7 9 133.19 16.10 -1 7 -9 164.28 15.00 4 -8 -9 6.20 6.60 4 -8 -9 4.90 7.00 -4 8 9 10.90 6.50 4 8 -9 -4.40 5.70 3 -8 -9 41.00 10.00 3 -8 -9 32.30 9.10 -3 8 9 29.80 8.50 3 8 -9 17.60 7.30 2 -8 -9 349.37 24.90 2 -8 -9 323.87 22.40 -2 8 9 343.87 23.80 2 8 -9 315.07 24.60 1 -8 -9 404.46 24.90 1 -8 -9 455.75 28.70 1 8 -9 434.06 28.20 -1 8 9 430.96 27.90 0 -8 -9 201.28 19.80 0 -8 -9 220.28 18.60 0 8 9 226.38 20.20 0 8 -9 181.98 13.60 0 8 -9 213.88 20.00 -1 -8 -9 16.90 7.20 -1 -8 -9 38.80 10.00 1 8 9 51.89 11.80 -1 8 -9 41.60 8.20 -1 8 -9 37.40 10.20 3 -9 -9 19.50 8.50 3 -9 -9 13.20 7.30 -3 9 9 25.70 8.40 3 9 -9 27.40 8.40 2 -9 -9 15.50 7.60 2 -9 -9 -7.70 4.70 -2 9 9 3.10 5.50 2 9 -9 6.20 6.60 1 -9 -9 23.10 9.20 1 -9 -9 23.30 8.60 1 9 -9 9.30 7.70 -1 9 9 17.00 7.50 0 -9 -9 8.00 7.00 0 -9 -9 1.10 5.70 0 9 -9 7.60 6.60 0 9 9 4.50 5.50 4 0 -10 52.29 9.90 -4 0 10 46.40 10.50 4 0 -10 40.50 7.30 4 0 -10 52.99 12.00 3 0 -10 134.79 10.00 3 0 -10 116.09 17.00 -3 0 10 119.49 14.40 3 0 -10 142.49 14.00 -2 0 10 792.62 39.40 2 0 -10 886.21 37.50 2 0 -10 825.12 28.90 -1 0 10 833.12 40.40 1 0 -10 925.21 36.80 1 0 -10 868.41 38.40 0 0 10 157.78 17.70 0 0 -10 150.78 15.90 4 -1 -10 72.09 12.00 -4 -1 10 65.09 11.80 4 -1 -10 62.09 13.00 4 -1 -10 50.09 8.50 4 1 -10 79.19 13.80 4 1 -10 80.39 11.90 -4 1 10 72.29 13.00 3 -1 -10 110.99 10.40 3 -1 -10 97.59 13.90 -3 -1 10 129.39 14.80 3 1 -10 114.69 13.10 -3 1 10 138.29 16.40 3 1 -10 108.79 16.80 2 -1 -10 -2.20 3.40 -2 -1 10 -0.90 4.90 2 -1 -10 -1.80 4.70 -2 1 10 9.20 5.60 1 -1 -10 65.89 9.10 -1 -1 10 66.79 12.60 1 -1 -10 45.10 10.00 -1 1 10 70.99 13.40 1 1 -10 57.79 11.00 0 -1 10 277.17 22.40 0 -1 -10 237.18 15.10 0 -1 -10 243.78 20.10 0 1 10 282.77 23.00 0 1 -10 261.97 20.60 -3 -2 10 -8.50 3.90 3 -2 -10 -4.90 5.10 3 -2 -10 6.30 5.40 3 2 -10 1.30 5.30 -3 2 10 8.20 6.60 3 2 -10 3.40 5.60 2 -2 -10 31.50 8.60 2 -2 -10 41.40 7.40 -2 -2 10 41.50 10.10 2 2 -10 42.70 9.80 -2 2 10 63.89 12.50 2 2 -10 28.30 8.80 -1 -2 10 104.69 15.60 1 -2 -10 55.19 11.60 1 -2 -10 84.29 9.80 1 2 -10 83.69 16.60 -1 2 10 57.79 12.30 0 -2 -10 8.50 5.50 0 -2 10 4.50 5.60 0 -2 -10 3.70 5.00 0 2 -10 -1.60 5.30 0 2 10 4.60 6.70 3 -3 -10 17.60 7.40 3 -3 -10 34.50 8.10 -3 -3 10 43.90 10.90 3 3 -10 41.20 11.30 3 3 -10 30.40 7.80 -3 3 10 64.59 11.90 2 -3 -10 -1.70 4.70 2 -3 -10 5.20 5.10 -2 -3 10 -1.10 5.00 2 3 -10 -1.40 4.80 -2 3 10 -5.40 4.80 2 3 -10 -0.90 4.30 1 -3 -10 9.90 6.50 -1 -3 10 12.10 7.70 1 -3 -10 2.60 5.50 -1 3 10 15.80 6.60 1 3 -10 17.90 7.00 1 3 -10 12.60 6.50 0 -3 -10 58.89 13.00 0 -3 10 99.39 15.40 0 -3 -10 80.49 11.50 0 3 10 66.59 13.30 0 3 -10 89.19 12.90 3 -4 -10 19.30 7.30 3 4 -10 19.00 7.60 3 4 -10 19.30 5.90 -3 4 10 11.80 6.80 -2 -4 10 304.57 23.60 2 -4 -10 225.98 17.20 2 -4 -10 241.48 20.10 2 4 -10 211.08 16.50 2 4 -10 261.67 22.90 -2 4 10 252.67 21.70 1 -4 -10 425.66 27.80 1 -4 -10 429.66 23.60 -1 -4 10 432.66 28.70 1 4 -10 437.66 29.90 1 4 -10 428.26 23.90 -1 4 10 422.16 28.30 0 -4 -10 16.40 7.30 0 -4 -10 17.70 6.90 0 -4 10 19.00 8.90 0 4 10 24.40 8.70 0 4 -10 8.70 7.20 0 4 -10 5.70 6.10 2 -5 -10 -4.20 4.90 -2 -5 10 -2.60 4.90 2 -5 -10 6.00 5.90 -2 5 10 8.80 6.20 2 5 -10 2.20 5.10 2 5 -10 -6.30 4.50 1 -5 -10 46.70 10.10 1 -5 -10 70.99 12.70 -1 -5 10 56.49 11.90 -1 5 10 62.89 11.90 1 5 -10 48.10 11.50 1 5 -10 51.59 9.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 54010 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.57062(3) 0.35544(2) 0.81230(3) 0.01620(8) Uani 1 1 d . . . . . C1 C -0.0661(2) 0.38268(11) 0.0536(2) 0.0176(3) Uani 1 1 d . . . . . O1 O 0.6340(2) 0.21691(9) 0.82050(18) 0.0259(3) Uani 1 1 d . . . . . H1 H 0.677(3) 0.2046(6) 0.909(3) 0.039 Uiso 1 1 calc R U . . . O2 O 0.76770(19) 0.37062(9) 0.64240(17) 0.0214(3) Uani 1 1 d . . . . . H2 H 0.762(2) 0.4217(16) 0.603(3) 0.032 Uiso 1 1 calc R U . . . C2 C 0.0384(2) 0.41984(12) 0.2231(2) 0.0237(4) Uani 1 1 d . . . . . H2A H 0.122493 0.465957 0.196520 0.028 Uiso 1 1 calc R U . . . H2AB H -0.047608 0.448406 0.287159 0.028 Uiso 1 1 calc R U . . . O4 O 0.38382(17) 0.33987(10) 0.98176(17) 0.0222(3) Uani 1 1 d . . . . . H4 H 0.300(3) 0.3536(16) 0.9421(19) 0.033 Uiso 1 1 calc R U . . . C4 C 0.2665(2) 0.38824(12) 0.4979(2) 0.0187(3) Uani 1 1 d . . . . . O3 O 0.5198(2) 0.49463(9) 0.79947(19) 0.0308(3) Uani 1 1 d . . . . . H3 H 0.435(4) 0.5051(4) 0.721(4) 0.046 Uiso 1 1 calc R U . . . C3 C 0.1457(3) 0.34913(12) 0.3385(2) 0.0239(4) Uani 1 1 d . . . . . H3A H 0.221805 0.315860 0.270506 0.029 Uiso 1 1 calc R U . . . H3AB H 0.060524 0.306792 0.376247 0.029 Uiso 1 1 calc R U . . . O5 O 0.2600(2) 0.47048(9) 0.52995(17) 0.0313(3) Uani 1 1 d . . . . . H5 H 0.384(4) 0.2886(19) 1.016(4) 0.052(8) Uiso 1 1 d . . . . . O7 O 0.01879(17) 0.36741(9) -0.06914(16) 0.0264(3) Uani 1 1 d . . . . . H7 H 0.524(4) 0.532(2) 0.871(4) 0.070(10) Uiso 1 1 d . . . . . O6 O 0.36957(17) 0.33277(8) 0.59383(15) 0.0229(3) Uani 1 1 d . . . . . H6 H 0.674(4) 0.1947(18) 0.749(4) 0.046(8) Uiso 1 1 d . . . . . O8 O -0.23775(16) 0.37165(9) 0.04229(15) 0.0244(3) Uani 1 1 d . . . . . H8 H 0.853(3) 0.3667(15) 0.708(3) 0.028(6) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01527(12) 0.01968(13) 0.01229(12) -0.00120(8) -0.00158(8) 0.00078(8) C1 0.0161(8) 0.0182(7) 0.0162(7) 0.0024(6) -0.0041(6) 0.0014(6) O1 0.0366(8) 0.0244(7) 0.0157(6) 0.0004(5) 0.0015(6) 0.0080(6) O2 0.0221(7) 0.0230(6) 0.0177(6) 0.0005(5) -0.0011(5) -0.0011(5) C2 0.0224(8) 0.0248(8) 0.0203(8) -0.0026(7) -0.0072(6) 0.0008(7) O4 0.0146(6) 0.0291(7) 0.0223(6) 0.0043(5) 0.0010(5) 0.0006(5) C4 0.0169(8) 0.0247(8) 0.0130(7) 0.0005(6) -0.0015(6) -0.0011(6) O3 0.0380(8) 0.0222(7) 0.0270(7) -0.0062(6) -0.0088(6) 0.0042(6) C3 0.0266(9) 0.0237(8) 0.0176(8) -0.0009(6) -0.0075(7) -0.0004(7) O5 0.0399(8) 0.0236(6) 0.0242(7) -0.0019(5) -0.0123(6) 0.0035(6) O7 0.0167(6) 0.0411(8) 0.0201(6) -0.0024(5) -0.0004(5) 0.0037(5) O6 0.0241(6) 0.0240(6) 0.0167(6) -0.0014(5) -0.0080(5) 0.0024(5) O8 0.0157(6) 0.0415(7) 0.0146(6) -0.0025(5) -0.0018(5) -0.0050(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Co1 O6 92.21(5) . . ? O4 Co1 O3 90.34(6) . . ? O6 Co1 O3 91.25(5) . . ? O4 Co1 O8 84.21(5) . 1_656 ? O6 Co1 O8 175.76(5) . 1_656 ? O3 Co1 O8 91.04(5) . 1_656 ? O4 Co1 O1 92.38(6) . . ? O6 Co1 O1 89.57(5) . . ? O3 Co1 O1 177.13(6) . . ? O8 Co1 O1 88.31(5) 1_656 . ? O4 Co1 O2 178.73(5) . . ? O6 Co1 O2 88.93(5) . . ? O3 Co1 O2 90.18(6) . . ? O8 Co1 O2 94.62(5) 1_656 . ? O1 Co1 O2 87.09(5) . . ? O7 C1 O8 123.43(15) . . ? O7 C1 C2 118.81(15) . . ? O8 C1 C2 117.72(15) . . ? Co1 O1 H1 109.5 . . ? Co1 O1 H6 121(2) . . ? H1 O1 H6 115.0 . . ? Co1 O2 H2 109.5 . . ? Co1 O2 H8 99.0(19) . . ? H2 O2 H8 108.3 . . ? C3 C2 C1 113.84(15) . . ? C3 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? C3 C2 H2AB 108.8 . . ? C1 C2 H2AB 108.8 . . ? H2A C2 H2AB 107.7 . . ? Co1 O4 H4 109.5 . . ? Co1 O4 H5 110.4(19) . . ? H4 O4 H5 112.9 . . ? O5 C4 O6 123.61(15) . . ? O5 C4 C3 119.98(15) . . ? O6 C4 C3 116.41(15) . . ? Co1 O3 H3 109.5 . . ? Co1 O3 H7 133(2) . . ? H3 O3 H7 109.4 . . ? C2 C3 C4 113.48(14) . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3AB 108.9 . . ? C4 C3 H3AB 108.9 . . ? H3A C3 H3AB 107.7 . . ? C4 O6 Co1 130.32(11) . . ? C1 O8 Co1 126.72(11) . 1_454 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O4 2.0791(12) . ? Co1 O6 2.0887(12) . ? Co1 O3 2.0955(14) . ? Co1 O8 2.1009(12) 1_656 ? Co1 O1 2.1038(13) . ? Co1 O2 2.1404(13) . ? C1 O7 1.249(2) . ? C1 O8 1.270(2) . ? C1 C2 1.515(2) . ? O1 H1 0.73(3) . ? O1 H6 0.75(3) . ? O2 H2 0.82(2) . ? O2 H8 0.74(3) . ? C2 C3 1.514(2) . ? C2 H2A 0.9700 . ? C2 H2AB 0.9700 . ? O4 H4 0.67(3) . ? O4 H5 0.81(3) . ? C4 O5 1.246(2) . ? C4 O6 1.274(2) . ? C4 C3 1.516(2) . ? O3 H3 0.81(3) . ? O3 H7 0.79(3) . ? C3 H3A 0.9700 . ? C3 H3AB 0.9700 . ?