#------------------------------------------------------------------------------ #$Date: 2025-08-19 20:21:09 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301810 $ #$URL: svn://www.crystallography.net/cod/cif/3/50/00/3500027.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_3500027 loop_ _publ_author_name 'Miguel Quir\'os' _publ_section_title ; Redetermination of mer-[Co(NH3)3(NO2)3] ; _journal_name_full 'Personal communication to COD' _journal_year 2016 _chemical_formula_moiety 'Co H9 N6 O6' _chemical_formula_sum 'Co H9 N6 O6' _chemical_formula_weight 248.06 _chemical_name_systematic mer-Tri(ammine)tri(nitrito-N)cobalt(III) _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens difmap _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.8358(3) _cell_length_b 10.0116(6) _cell_length_c 11.6421(6) _cell_measurement_reflns_used 3899 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.71 _cell_measurement_theta_min 2.68 _cell_volume 796.75(7) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_unetI/netI 0.0384 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 5745 _diffrn_reflns_point_group_measured_fraction_full 0.965 _diffrn_reflns_point_group_measured_fraction_max 0.942 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.704 _diffrn_reflns_theta_min 2.683 _exptl_absorpt_coefficient_mu 2.173 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_correction_T_min 0.615 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.068 _exptl_crystal_description prismatic _exptl_crystal_F_000 504 _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.160 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _refine_diff_density_max 0.360 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.084 _refine_ls_abs_structure_details ; Flack x determined using 671 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.011(15) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 121 _refine_ls_number_reflns 1951 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.106 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0264 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.1200P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.0544 _reflns_Friedel_coverage 0.631 _reflns_Friedel_fraction_full 0.928 _reflns_Friedel_fraction_max 0.883 _reflns_number_gt 1821 _reflns_number_total 1951 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file merco.cif _cod_data_source_block merco _cod_database_code 3500027 _cod_database_fobs_code 3500027 _shelx_shelxl_version_number 2014/7 _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_estimated_absorpt_t_min 0.624 _shelx_estimated_absorpt_t_max 0.722 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 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 Co Co 0.24073(5) 0.68271(3) 0.25718(3) 0.00415(10) Uani 1 1 d . . . . . N1N N 0.0392(4) 0.6394(3) 0.3682(2) 0.0086(5) Uani 1 1 d . . . . . O1 O -0.1088(3) 0.5756(2) 0.33963(19) 0.0150(5) Uani 1 1 d . . . . . O2 O 0.0579(4) 0.6756(2) 0.46969(17) 0.0160(5) Uani 1 1 d . . . . . N2N N 0.4395(4) 0.7234(3) 0.1455(2) 0.0081(5) Uani 1 1 d . . . . . O3 O 0.4253(3) 0.8279(2) 0.08789(17) 0.0115(4) Uani 1 1 d . . . . . O4 O 0.5785(3) 0.6466(2) 0.1302(2) 0.0164(5) Uani 1 1 d . . . . . N3N N 0.2102(4) 0.5073(2) 0.18778(19) 0.0074(5) Uani 1 1 d . . . . . O5 O 0.2899(3) 0.4075(2) 0.23073(17) 0.0120(4) Uani 1 1 d . . . . . O6 O 0.1060(3) 0.4928(2) 0.10200(17) 0.0149(5) Uani 1 1 d . . . . . N1M N 0.0439(4) 0.7566(3) 0.1529(2) 0.0095(6) Uani 1 1 d . . . . . H1A H 0.0247 0.7002 0.0948 0.011 Uiso 1 1 d R U . . . H1B H -0.0679 0.7685 0.1907 0.011 Uiso 1 1 d R U . . . H1C H 0.0856 0.8346 0.1257 0.011 Uiso 1 1 d R U . . . N2M N 0.2742(4) 0.8597(2) 0.32737(19) 0.0076(5) Uani 1 1 d . . . . . H2A H 0.2421 0.9226 0.2766 0.009 Uiso 1 1 d R U . . . H2B H 0.1971 0.8665 0.3887 0.009 Uiso 1 1 d R U . . . H2C H 0.3983 0.8704 0.3485 0.009 Uiso 1 1 d R U . . . N3M N 0.4360(4) 0.6145(3) 0.3634(2) 0.0086(5) Uani 1 1 d . . . . . H3A H 0.5531 0.6465 0.3443 0.010 Uiso 1 1 d R U . . . H3B H 0.4064 0.6402 0.4345 0.010 Uiso 1 1 d R U . . . H3C H 0.4382 0.5257 0.3601 0.010 Uiso 1 1 d R U . . . 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 Co 0.00352(16) 0.00570(16) 0.00322(15) -0.00020(13) 0.00037(19) -0.00020(14) N1N 0.0078(12) 0.0079(12) 0.0100(13) 0.0005(10) 0.0005(10) 0.0015(10) O1 0.0087(12) 0.0179(12) 0.0182(11) -0.0038(9) 0.0028(9) -0.0061(10) O2 0.0181(12) 0.0207(12) 0.0091(10) -0.0034(10) 0.0052(9) -0.0018(11) N2N 0.0099(13) 0.0085(12) 0.0060(12) -0.0012(10) -0.0011(10) -0.0029(10) O3 0.0172(11) 0.0085(10) 0.0088(9) 0.0034(9) 0.0011(8) -0.0018(9) O4 0.0109(12) 0.0160(12) 0.0224(12) 0.0019(9) 0.0083(10) 0.0050(9) N3N 0.0052(12) 0.0104(11) 0.0066(10) -0.0004(9) 0.0030(9) -0.0015(10) O5 0.0149(11) 0.0079(9) 0.0132(9) 0.0028(7) -0.0018(9) 0.0020(8) O6 0.0193(13) 0.0148(11) 0.0108(11) -0.0045(9) -0.0070(9) 0.0013(10) N1M 0.0091(13) 0.0093(13) 0.0101(13) 0.0004(10) -0.0010(11) 0.0001(10) N2M 0.0069(12) 0.0090(11) 0.0071(10) -0.0012(8) 0.0001(10) -0.0005(10) N3M 0.0092(13) 0.0101(13) 0.0065(12) -0.0008(10) 0.0006(11) 0.0002(10) 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' N N 0.0061 0.0033 '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' Co Co 0.3494 0.9721 '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 N2N Co N1N 179.13(11) . . N2N Co N3M 91.11(11) . . N1N Co N3M 89.16(10) . . N2N Co N3N 89.21(10) . . N1N Co N3N 89.95(10) . . N3M Co N3N 91.20(10) . . N2N Co N1M 89.20(10) . . N1N Co N1M 90.56(11) . . N3M Co N1M 178.21(11) . . N3N Co N1M 90.56(10) . . N2N Co N2M 90.45(11) . . N1N Co N2M 90.39(11) . . N3M Co N2M 88.40(10) . . N3N Co N2M 179.48(11) . . N1M Co N2M 89.83(11) . . O2 N1N O1 119.3(3) . . O2 N1N Co 119.7(2) . . O1 N1N Co 121.0(2) . . O4 N2N O3 120.3(3) . . O4 N2N Co 120.6(2) . . O3 N2N Co 119.1(2) . . O6 N3N O5 118.9(2) . . O6 N3N Co 120.2(2) . . O5 N3N Co 120.78(18) . . Co N1M H1A 109.4 . . Co N1M H1B 109.5 . . H1A N1M H1B 109.5 . . Co N1M H1C 109.4 . . H1A N1M H1C 109.5 . . H1B N1M H1C 109.5 . . Co N2M H2A 109.4 . . Co N2M H2B 109.5 . . H2A N2M H2B 109.5 . . Co N2M H2C 109.5 . . H2A N2M H2C 109.5 . . H2B N2M H2C 109.5 . . Co N3M H3A 109.4 . . Co N3M H3B 109.5 . . H3A N3M H3B 109.5 . . Co N3M H3C 109.5 . . H3A N3M H3C 109.5 . . H3B N3M H3C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Co N2N 1.924(3) . Co N1N 1.938(3) . Co N3M 1.944(3) . Co N3N 1.944(2) . Co N1M 1.957(3) . Co N2M 1.965(2) . N1N O2 1.242(3) . N1N O1 1.242(4) . N2N O4 1.235(4) . N2N O3 1.246(3) . N3N O6 1.235(3) . N3N O5 1.243(3) . N1M H1A 0.8900 . N1M H1B 0.8900 . N1M H1C 0.8900 . N2M H2A 0.8902 . N2M H2B 0.8902 . N2M H2C 0.8902 . N3M H3A 0.8900 . N3M H3B 0.8900 . N3M H3C 0.8900 . loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 24202142