#------------------------------------------------------------------------------ #$Date: 2016-02-21 00:03:34 +0000 (Sun, 21 Feb 2016) $ #$Revision: 176798 $ #$URL: svn://www.crystallography.net/cod/cif/2/23/90/2239011.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_2239011 loop_ _publ_author_name 'Waldhart, Greyson W.' 'Mankad, Neal P.' _publ_section_title ; trans-Tetracarbonylbis(triphenylphosphane-\kP)molybdenum(0) ; _journal_coeditor_code PJ2007 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m36 _journal_paper_doi 10.1107/S1600536814000300 _journal_volume 70 _journal_year 2014 _chemical_formula_iupac '[Mo (C18 H15 P)2 (C O)4]' _chemical_formula_sum 'C40 H30 Mo O4 P2' _chemical_formula_weight 732.52 _chemical_name_common trans-Mo(CO)4(PPh3)2 _chemical_name_systematic ; trans-Tetracarbonylbis(triphenylphosphane-\kP)molybdenum(0) ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 64.794(4) _cell_angle_beta 69.417(4) _cell_angle_gamma 83.699(4) _cell_formula_units_Z 1 _cell_length_a 9.3443(13) _cell_length_b 10.2267(15) _cell_length_c 10.7258(16) _cell_measurement_reflns_used 6345 _cell_measurement_temperature 300.(2) _cell_measurement_theta_max 25.0596 _cell_measurement_theta_min 2.2004 _cell_volume 867.2(2) _computing_cell_refinement 'SAINT (Bruker, 2013)' _computing_data_collection 'SMART (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2013)' _computing_molecular_graphics 'Mercury (Macrae et al., 2006)' _computing_publication_material 'publCIF (Westrip, 2010)' _computing_structure_refinement 'SHELXL2013 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 300.(2) _diffrn_detector_area_resol_mean 8.3330 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Bruker SMART X2S benchtop' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator 'doubly curved silicon crystal' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 7865 _diffrn_reflns_theta_full 24.72 _diffrn_reflns_theta_max 24.72 _diffrn_reflns_theta_min 2.33 _exptl_absorpt_coefficient_mu 0.511 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2012)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 374 _exptl_crystal_size_max 0.620 _exptl_crystal_size_mid 0.450 _exptl_crystal_size_min 0.330 _refine_diff_density_max 0.247 _refine_diff_density_min -0.281 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 214 _refine_ls_number_reflns 2907 _refine_ls_number_restraints 61 _refine_ls_restrained_S_all 1.095 _refine_ls_R_factor_all 0.0238 _refine_ls_R_factor_gt 0.0220 _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^)+(0.0238P)^2^+0.3878P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.0575 _reflns_number_gt 2770 _reflns_number_total 2907 _reflns_threshold_expression I>2\s(I) _cod_data_source_file pj2007sup1.cif _cod_data_source_block I _cod_database_code 2239011 _cod_database_fobs_code 2239011 #BEGIN Tags that were not found in dictionaries: _shelx_hkl_checksum 3420 _shelx_hkl_file ; -1 0 0 105.18 2.54 -1 0 0 116.19 2.54 1 0 0 108.46 2.54 -2 0 0 67.96 1.64 -2 0 0 68.82 1.65 2 0 0 64.75 1.64 2 0 0 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0.42 9 -3 0 3.39 0.38 -9 3 0 2.44 0.34 8 -3 0 21.04 0.81 -8 3 0 20.60 0.84 7 -3 0 31.89 1.01 -7 3 0 31.40 1.05 6 -3 0 21.09 0.71 -6 3 0 20.68 0.75 5 -3 0 4.35 0.26 -5 3 0 4.77 0.32 -5 3 0 5.01 0.19 -5 3 0 4.59 0.19 4 -3 0 3.41 0.17 4 -3 0 3.23 0.19 4 -3 0 2.73 0.24 -4 3 0 2.98 0.15 -4 3 0 2.73 0.19 3 -3 0 322.11 7.06 3 -3 0 307.57 7.33 3 -3 0 307.81 7.20 -3 3 0 320.58 7.21 -3 3 0 309.78 7.05 2 -3 0 118.28 2.77 2 -3 0 122.95 2.76 2 -3 0 114.16 2.88 -2 3 0 120.34 2.78 -2 3 0 118.75 2.75 1 -3 0 66.09 1.59 1 -3 0 66.42 1.58 1 -3 0 64.13 1.66 -1 3 0 66.55 1.59 -1 3 0 64.56 1.66 -1 3 0 68.60 1.58 0 -3 0 0.39 0.09 0 -3 0 0.43 0.08 0 -3 0 0.30 0.06 0 3 0 0.35 0.07 0 3 0 0.28 0.08 -1 -3 0 15.29 0.51 -1 -3 0 15.22 0.48 1 3 0 15.76 0.49 1 3 0 16.50 0.48 -2 -3 0 310.08 6.92 -2 -3 0 301.85 7.15 2 3 0 304.99 6.92 2 3 0 307.00 7.12 -3 -3 0 273.53 6.60 3 3 0 284.83 6.37 3 3 0 283.25 6.60 -4 -3 0 1.91 0.21 4 3 0 1.73 0.20 -5 -3 0 2.75 0.26 5 3 0 2.65 0.19 5 3 0 3.06 0.29 -6 -3 0 28.20 0.95 6 3 0 27.54 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9.84 0.72 -1 4 11 9.29 0.60 0 -4 -11 0.46 0.27 0 4 11 0.33 0.22 0 4 11 0.52 0.27 -1 -4 -11 7.87 0.60 1 4 11 7.27 0.56 1 4 11 6.83 0.57 -2 -4 -11 27.41 1.11 2 4 11 26.63 1.03 2 4 11 27.94 1.05 -3 -4 -11 24.82 1.08 3 4 11 29.04 1.08 -4 -4 -11 8.75 0.61 4 4 11 9.49 0.62 -5 -4 -11 2.23 0.36 5 4 11 2.69 0.36 -6 -4 -11 21.81 0.96 6 4 11 20.60 0.95 -7 -4 -11 38.12 1.37 7 4 11 36.97 1.35 -8 -4 -11 18.31 0.92 8 4 11 19.66 0.93 1 -5 -11 0.90 0.29 -1 5 11 0.75 0.24 -1 5 11 1.19 0.32 0 -5 -11 15.28 0.84 0 5 11 14.92 0.75 0 5 11 15.01 0.82 -1 -5 -11 49.53 1.69 1 5 11 49.49 1.64 1 5 11 53.41 1.60 -2 -5 -11 18.89 0.92 2 5 11 19.07 0.84 2 5 11 18.42 0.82 -3 -5 -11 12.62 0.73 3 5 11 12.53 0.70 -4 -5 -11 11.48 0.71 4 5 11 10.69 0.66 -5 -5 -11 16.77 0.86 5 5 11 17.77 0.85 -6 -5 -11 62.26 1.97 6 5 11 62.78 1.92 -7 -5 -11 18.10 0.91 7 5 11 18.38 0.90 -8 -5 -11 7.28 0.62 8 5 11 7.40 0.61 1 -6 -11 3.42 0.46 -1 6 11 4.51 0.46 -1 6 11 4.24 0.49 0 -6 -11 17.77 0.94 0 6 11 15.66 0.85 0 6 11 18.14 0.81 -1 -6 -11 30.18 1.21 1 6 11 28.16 1.06 1 6 11 27.14 1.09 -2 -6 -11 24.94 1.07 2 6 11 23.61 0.95 2 6 11 24.95 0.99 -3 -6 -11 15.67 0.83 3 6 11 16.23 0.78 -4 -6 -11 3.80 0.45 4 6 11 3.79 0.42 -5 -6 -11 13.21 0.80 5 6 11 13.90 0.75 -6 -6 -11 30.71 1.23 6 6 11 28.74 1.15 -7 -6 -11 1.45 0.33 7 6 11 1.99 0.34 -8 -6 -11 5.26 0.57 8 6 11 6.02 0.59 1 -7 -11 5.30 0.56 -1 7 11 3.36 0.39 -1 7 11 3.19 0.45 0 -7 -11 16.99 0.91 0 7 11 17.38 0.80 0 7 11 15.85 0.85 1 7 11 18.34 0.87 1 7 11 21.13 0.88 -2 -7 -11 3.93 0.48 2 7 11 4.20 0.44 2 7 11 4.36 0.46 -3 -7 -11 2.05 0.38 3 7 11 1.43 0.30 -4 -7 -11 3.29 0.43 4 7 11 3.55 0.41 -5 -7 -11 12.15 0.77 5 7 11 11.32 0.68 -6 -7 -11 12.69 0.81 6 7 11 14.61 0.78 -7 -7 -11 0.41 0.28 7 7 11 0.82 0.28 0 -8 -11 8.19 0.69 0 8 11 7.22 0.60 0 8 11 7.51 0.55 -1 -8 -11 1.82 0.38 1 8 11 1.87 0.32 1 8 11 1.97 0.32 -2 -8 -11 0.11 0.24 2 8 11 -0.15 0.17 2 8 11 0.10 0.21 -3 -8 -11 7.04 0.64 3 8 11 7.05 0.55 -4 -8 -11 21.22 1.04 4 8 11 21.13 0.94 -5 -8 -11 18.37 1.00 5 8 11 18.43 0.88 -6 -8 -11 0.42 0.30 6 8 11 1.17 0.31 -1 -9 -11 -0.17 0.23 1 9 11 -0.14 0.19 1 9 11 0.19 0.23 -2 -9 -11 0.16 0.27 2 9 11 0.25 0.21 -3 -9 -11 31.80 1.37 3 9 11 34.87 1.25 -4 -9 -11 18.78 1.01 4 9 11 19.04 0.88 -5 -9 -11 0.22 0.28 5 9 11 0.32 0.23 -3 -2 -12 0.24 0.27 3 2 12 0.77 0.28 -4 -2 -12 14.73 0.80 4 2 12 16.07 0.85 -5 -2 -12 29.73 1.15 5 2 12 29.78 1.21 -2 -3 -12 1.36 0.33 2 3 12 1.78 0.34 2 3 12 1.45 0.33 -3 -3 -12 13.91 0.80 3 3 12 14.18 0.79 -4 -3 -12 37.72 1.41 4 3 12 41.02 1.43 -5 -3 -12 23.95 1.05 5 3 12 25.24 1.07 -6 -3 -12 3.42 0.44 6 3 12 4.07 0.46 -1 -4 -12 1.06 0.33 1 4 12 1.35 0.34 1 4 12 1.75 0.34 -2 -4 -12 17.84 0.94 2 4 12 19.38 0.89 2 4 12 18.51 0.92 -3 -4 -12 22.52 1.04 3 4 12 22.34 0.99 -4 -4 -12 23.07 1.09 4 4 12 27.46 1.10 -5 -4 -12 4.17 0.47 5 4 12 5.01 0.52 -6 -4 -12 1.10 0.33 6 4 12 0.65 0.30 -1 -5 -12 17.67 0.94 1 5 12 16.94 0.84 1 5 12 16.40 0.86 -2 -5 -12 9.53 0.71 2 5 12 8.76 0.62 -3 -5 -12 7.71 0.65 3 5 12 7.66 0.61 -4 -5 -12 8.83 0.66 4 5 12 10.47 0.67 -5 -5 -12 0.56 0.27 5 5 12 0.62 0.26 -6 -5 -12 10.09 0.70 6 5 12 10.47 0.73 -1 -6 -12 8.11 0.68 1 6 12 9.20 0.63 1 6 12 7.93 0.64 -2 -6 -12 15.62 0.89 2 6 12 14.41 0.78 -3 -6 -12 6.36 0.59 3 6 12 6.10 0.57 -4 -6 -12 -0.22 0.22 4 6 12 0.46 0.25 -5 -6 -12 2.90 0.44 5 6 12 3.21 0.41 -6 -6 -12 18.13 0.97 6 6 12 18.71 0.92 -2 -7 -12 8.88 0.77 2 7 12 12.90 0.72 -3 -7 -12 0.50 0.29 3 7 12 0.13 0.24 -4 -7 -12 2.65 0.42 4 7 12 2.43 0.36 -5 -7 -12 6.70 0.63 5 7 12 7.30 0.61 -6 -7 -12 12.36 0.82 6 7 12 12.10 0.76 -3 -8 -12 0.70 0.32 3 8 12 0.82 0.28 -4 -8 -12 3.62 0.49 4 8 12 3.60 0.45 0 0 0 0.00 0.00 ; _shelx_res_checksum 80316 _shelx_res_file ; TITL scan_0m_P1 in P1 CELL 0.71073 9.3443 10.2267 10.7258 64.794 69.417 83.699 ZERR 1.00 0.0013 0.0015 0.0016 0.004 0.004 0.004 LATT 1 SFAC C H O P MO UNIT 40 30 4 2 1 MERG 2 OMIT 0 1 0 OMIT 0 0 1 SHEL 999 0.839 DELU FMAP 2 PLAN 10 SIZE 0.330 0.450 0.620 ACTA BOND $H L.S. 22 TEMP 27.00 WGHT 0.023800 0.387800 FVAR 0.32772 MO1 5 0.000000 0.000000 1.000000 10.50000 0.02853 0.02430 = 0.02774 -0.00693 -0.00954 -0.00060 P1 4 0.213945 0.168937 0.798654 11.00000 0.02881 0.02605 = 0.02904 -0.00910 -0.00896 -0.00119 O1 3 0.007788 0.137439 1.213199 11.00000 0.06993 0.08220 = 0.06636 -0.04966 -0.02230 0.00037 O2 3 0.251687 -0.220320 1.087911 11.00000 0.06754 0.06062 = 0.06943 -0.01970 -0.03455 0.03155 C1 1 0.006545 0.088633 1.135534 11.00000 0.03548 0.04019 = 0.04057 -0.01502 -0.01151 -0.00054 C2 1 0.159425 -0.142548 1.058475 11.00000 0.04320 0.03511 = 0.03581 -0.01000 -0.01295 0.00270 C5 1 0.259068 0.310939 0.842518 11.00000 0.03468 0.03554 = 0.03526 -0.01562 -0.00574 -0.00542 C6 1 0.327424 0.276888 0.947822 11.00000 0.05990 0.04853 = 0.04772 -0.01697 -0.01956 -0.01083 AFIX 43 H6 2 0.358231 0.183355 0.989954 11.00000 -1.20000 AFIX 0 C7 1 0.350158 0.380023 0.990640 11.00000 0.07013 0.07820 = 0.05248 -0.03105 -0.01671 -0.02447 AFIX 43 H7 2 0.397581 0.355674 1.060192 11.00000 -1.20000 AFIX 0 C8 1 0.304270 0.516367 0.932650 11.00000 0.08776 0.07383 = 0.07783 -0.05310 -0.01061 -0.01875 AFIX 43 H8 2 0.320109 0.585503 0.961909 11.00000 -1.20000 AFIX 0 C9 1 0.234396 0.551386 0.830622 11.00000 0.10954 0.05200 = 0.11527 -0.05373 -0.04628 0.01935 AFIX 43 H9 2 0.201351 0.644534 0.791512 11.00000 -1.20000 AFIX 0 C10 1 0.212249 0.449615 0.784814 11.00000 0.07422 0.04792 = 0.07866 -0.03786 -0.03792 0.01717 AFIX 43 H10 2 0.165445 0.475256 0.714631 11.00000 -1.20000 AFIX 0 C11 1 0.398908 0.088574 0.743421 11.00000 0.03296 0.03875 = 0.03535 -0.01221 -0.01020 0.00377 C12 1 0.398793 -0.033783 0.719501 11.00000 0.04705 0.05241 = 0.05989 -0.03142 -0.01014 0.00432 AFIX 43 H12 2 0.305926 -0.075131 0.737092 11.00000 -1.20000 AFIX 0 C13 1 0.532372 -0.096191 0.670339 11.00000 0.06934 0.06525 = 0.07132 -0.03989 -0.01592 0.02195 AFIX 43 H13 2 0.528916 -0.177210 0.652879 11.00000 -1.20000 AFIX 0 C14 1 0.667709 -0.040668 0.647451 11.00000 0.05681 0.09890 = 0.08688 -0.05081 -0.02211 0.03813 AFIX 43 H14 2 0.757777 -0.084413 0.616743 11.00000 -1.20000 AFIX 0 C15 1 0.671954 0.079506 0.669444 11.00000 0.03321 0.13563 = 0.15126 -0.08511 -0.02806 0.01422 AFIX 43 H15 2 0.765908 0.119035 0.651635 11.00000 -1.20000 AFIX 0 C16 1 0.538089 0.145163 0.718309 11.00000 0.03787 0.08464 = 0.11426 -0.06201 -0.01855 0.00308 AFIX 43 H16 2 0.543079 0.227088 0.733851 11.00000 -1.20000 AFIX 0 C17 1 0.195315 0.273529 0.616892 11.00000 0.04205 0.02867 = 0.02814 -0.00936 -0.00911 0.00269 C18 1 0.311992 0.369858 0.502418 11.00000 0.05342 0.05029 = 0.04103 -0.00802 -0.00672 -0.00766 AFIX 43 H18 2 0.400801 0.382215 0.517433 11.00000 -1.20000 AFIX 0 C19 1 0.297053 0.447353 0.366565 11.00000 0.07971 0.05063 = 0.03445 -0.00064 0.00126 -0.00254 AFIX 43 H19 2 0.375060 0.512811 0.291180 11.00000 -1.20000 AFIX 0 C20 1 0.167641 0.428357 0.342059 11.00000 0.09164 0.05772 = 0.03271 -0.00789 -0.02125 0.01550 AFIX 43 H20 2 0.157581 0.481341 0.250645 11.00000 -1.20000 AFIX 0 C21 1 0.054989 0.332229 0.451536 11.00000 0.07774 0.06974 = 0.04700 -0.00971 -0.03621 0.00551 AFIX 43 H21 2 -0.031624 0.317351 0.434620 11.00000 -1.20000 AFIX 0 C22 1 0.068133 0.255548 0.589284 11.00000 0.05204 0.04960 = 0.03608 -0.00623 -0.01858 -0.00417 AFIX 43 H22 2 -0.010880 0.190859 0.664052 11.00000 -1.20000 AFIX 0 HKLF 4 REM scan_0m_P1 in P1 REM R1 = 0.0220 for 2770 Fo > 4sig(Fo) and 0.0238 for all 2907 data REM 214 parameters refined using 61 restraints END WGHT 0.0238 0.3877 REM Highest difference peak 0.247, deepest hole -0.281, 1-sigma level 0.047 Q1 1 0.2408 0.2511 0.8122 11.00000 0.05 0.25 Q2 1 0.2045 0.2213 0.6951 11.00000 0.05 0.23 Q3 1 0.6836 0.0521 0.5992 11.00000 0.05 0.21 Q4 1 0.3174 0.1169 0.7738 11.00000 0.05 0.21 Q5 1 0.5356 0.2383 0.6794 11.00000 0.05 0.17 Q6 1 0.2606 0.4067 0.3488 11.00000 0.05 0.16 Q7 1 0.6617 0.1610 0.6366 11.00000 0.05 0.15 Q8 1 0.1108 0.4390 0.8020 11.00000 0.05 0.15 Q9 1 0.6004 -0.0318 0.6260 11.00000 0.05 0.15 Q10 1 0.2836 -0.0256 0.6596 11.00000 0.05 0.15 ; #END Tags that were not found in dictionaries loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy Mo Mo1 0 0 1.0 0.02814(8) Uani d 1 P P1 0.21394(5) 0.16894(5) 0.79865(5) 0.02888(12) Uani d 1 O O1 0.0078(2) 0.1374(2) 1.21320(19) 0.0659(5) Uani d 1 O O2 0.2517(2) -0.22032(19) 1.0879(2) 0.0677(5) Uani d 1 C C1 0.0065(2) 0.0886(2) 1.1355(2) 0.0396(4) Uani d 1 C C2 0.1594(2) -0.1425(2) 1.0585(2) 0.0400(4) Uani d 1 C C5 0.2591(2) 0.3109(2) 0.8425(2) 0.0360(4) Uani d 1 C C6 0.3274(3) 0.2769(3) 0.9478(2) 0.0516(5) Uani d 1 H H6 0.3582 0.1834 0.99 0.062 Uiso calc 1 C C7 0.3502(3) 0.3800(3) 0.9906(3) 0.0643(7) Uani d 1 H H7 0.3976 0.3557 1.0602 0.077 Uiso calc 1 C C8 0.3043(4) 0.5164(3) 0.9327(3) 0.0750(8) Uani d 1 H H8 0.3201 0.5855 0.9619 0.09 Uiso calc 1 C C9 0.2344(4) 0.5514(3) 0.8306(4) 0.0842(9) Uani d 1 H H9 0.2014 0.6445 0.7915 0.101 Uiso calc 1 C C10 0.2122(3) 0.4496(3) 0.7848(3) 0.0604(6) Uani d 1 H H10 0.1654 0.4753 0.7146 0.072 Uiso calc 1 C C11 0.3989(2) 0.0886(2) 0.7434(2) 0.0375(4) Uani d 1 C C12 0.3988(3) -0.0338(2) 0.7195(3) 0.0527(6) Uani d 1 H H12 0.3059 -0.0751 0.7371 0.063 Uiso calc 1 C C13 0.5324(3) -0.0962(3) 0.6703(3) 0.0684(7) Uani d 1 H H13 0.5289 -0.1772 0.6529 0.082 Uiso calc 1 C C14 0.6677(3) -0.0407(4) 0.6475(3) 0.0800(9) Uani d 1 H H14 0.7578 -0.0844 0.6167 0.096 Uiso calc 1 C C15 0.6720(3) 0.0795(4) 0.6694(4) 0.0992(12) Uani d 1 H H15 0.7659 0.119 0.6516 0.119 Uiso calc 1 C C16 0.5381(3) 0.1452(3) 0.7183(4) 0.0735(8) Uani d 1 H H16 0.5431 0.2271 0.7339 0.088 Uiso calc 1 C C17 0.1953(2) 0.27353(19) 0.61689(19) 0.0348(4) Uani d 1 C C18 0.3120(3) 0.3699(2) 0.5024(2) 0.0542(6) Uani d 1 H H18 0.4008 0.3822 0.5174 0.065 Uiso calc 1 C C19 0.2971(3) 0.4474(3) 0.3666(3) 0.0668(7) Uani d 1 H H19 0.3751 0.5128 0.2912 0.08 Uiso calc 1 C C20 0.1676(4) 0.4284(3) 0.3421(2) 0.0657(7) Uani d 1 H H20 0.1576 0.4813 0.2506 0.079 Uiso calc 1 C C21 0.0550(3) 0.3322(3) 0.4515(3) 0.0659(7) Uani d 1 H H21 -0.0316 0.3174 0.4346 0.079 Uiso calc 1 C C22 0.0681(3) 0.2555(2) 0.5893(2) 0.0485(5) Uani d 1 H H22 -0.0109 0.1909 0.6641 0.058 Uiso calc 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mo1 0.02853(13) 0.02430(12) 0.02774(12) -0.00060(8) -0.00954(9) -0.00693(9) P1 0.0288(3) 0.0261(2) 0.0290(2) -0.00119(18) -0.00896(19) -0.00910(19) O1 0.0699(12) 0.0822(12) 0.0664(11) 0.0004(9) -0.0223(9) -0.0497(10) O2 0.0675(11) 0.0606(10) 0.0694(11) 0.0316(9) -0.0346(10) -0.0197(9) C1 0.0355(11) 0.0402(11) 0.0406(11) -0.0005(8) -0.0115(9) -0.0150(9) C2 0.0432(12) 0.0351(10) 0.0358(10) 0.0027(9) -0.0130(9) -0.0100(8) C5 0.0347(10) 0.0355(10) 0.0353(10) -0.0054(8) -0.0057(8) -0.0156(8) C6 0.0599(14) 0.0485(12) 0.0477(12) -0.0108(10) -0.0196(11) -0.0170(10) C7 0.0701(17) 0.0782(18) 0.0525(14) -0.0245(14) -0.0167(12) -0.0311(13) C8 0.088(2) 0.0738(19) 0.0778(19) -0.0188(15) -0.0106(16) -0.0531(16) C9 0.110(3) 0.0520(16) 0.115(3) 0.0194(16) -0.046(2) -0.0537(17) C10 0.0742(17) 0.0479(13) 0.0787(17) 0.0172(12) -0.0379(14) -0.0379(13) C11 0.0330(10) 0.0387(10) 0.0354(10) 0.0038(8) -0.0102(8) -0.0122(8) C12 0.0471(13) 0.0524(13) 0.0599(14) 0.0043(10) -0.0101(11) -0.0314(11) C13 0.0693(18) 0.0652(16) 0.0713(17) 0.0220(13) -0.0159(14) -0.0399(14) C14 0.0568(17) 0.099(2) 0.087(2) 0.0381(16) -0.0221(15) -0.0508(19) C15 0.0332(14) 0.136(3) 0.151(3) 0.0142(17) -0.0281(18) -0.085(3) C16 0.0379(13) 0.0846(19) 0.114(2) 0.0031(12) -0.0185(14) -0.0620(19) C17 0.0421(11) 0.0287(9) 0.0281(9) 0.0027(8) -0.0091(8) -0.0094(7) C18 0.0534(14) 0.0503(13) 0.0410(12) -0.0077(10) -0.0067(10) -0.0080(10) C19 0.0797(19) 0.0506(14) 0.0345(12) -0.0025(13) 0.0013(12) -0.0006(10) C20 0.092(2) 0.0577(15) 0.0327(12) 0.0155(14) -0.0212(13) -0.0079(11) C21 0.0777(18) 0.0697(16) 0.0470(13) 0.0055(14) -0.0362(13) -0.0097(12) C22 0.0520(13) 0.0496(12) 0.0361(11) -0.0042(10) -0.0186(10) -0.0062(9) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle C1 Mo1 C1 . 2_557 180.00(11) C1 Mo1 C2 . 2_557 89.09(8) C1 Mo1 C2 2_557 2_557 90.91(8) C1 Mo1 C2 . . 90.91(8) C1 Mo1 C2 2_557 . 89.09(8) C2 Mo1 C2 2_557 . 180.0 C1 Mo1 P1 . 2_557 89.67(6) C1 Mo1 P1 2_557 2_557 90.33(6) C2 Mo1 P1 2_557 2_557 87.97(6) C2 Mo1 P1 . 2_557 92.03(6) C1 Mo1 P1 . . 90.33(6) C1 Mo1 P1 2_557 . 89.67(6) C2 Mo1 P1 2_557 . 92.04(6) C2 Mo1 P1 . . 87.97(6) P1 Mo1 P1 2_557 . 180.0 C5 P1 C11 . . 104.37(9) C5 P1 C17 . . 102.38(9) C11 P1 C17 . . 99.19(9) C5 P1 Mo1 . . 112.63(6) C11 P1 Mo1 . . 116.61(6) C17 P1 Mo1 . . 119.47(6) O1 C1 Mo1 . . 178.84(18) O2 C2 Mo1 . . 178.21(19) C10 C5 C6 . . 117.94(19) C10 C5 P1 . . 121.47(16) C6 C5 P1 . . 120.24(16) C7 C6 C5 . . 120.8(2) C7 C6 H6 . . 119.6 C5 C6 H6 . . 119.6 C8 C7 C6 . . 120.8(3) C8 C7 H7 . . 119.6 C6 C7 H7 . . 119.6 C7 C8 C9 . . 119.3(2) C7 C8 H8 . . 120.3 C9 C8 H8 . . 120.3 C8 C9 C10 . . 120.7(3) C8 C9 H9 . . 119.6 C10 C9 H9 . . 119.6 C5 C10 C9 . . 120.4(2) C5 C10 H10 . . 119.8 C9 C10 H10 . . 119.8 C16 C11 C12 . . 117.4(2) C16 C11 P1 . . 124.63(17) C12 C11 P1 . . 117.92(16) C13 C12 C11 . . 121.8(2) C13 C12 H12 . . 119.1 C11 C12 H12 . . 119.1 C14 C13 C12 . . 120.3(3) C14 C13 H13 . . 119.9 C12 C13 H13 . . 119.9 C13 C14 C15 . . 119.4(3) C13 C14 H14 . . 120.3 C15 C14 H14 . . 120.3 C14 C15 C16 . . 121.2(3) C14 C15 H15 . . 119.4 C16 C15 H15 . . 119.4 C11 C16 C15 . . 119.8(3) C11 C16 H16 . . 120.1 C15 C16 H16 . . 120.1 C22 C17 C18 . . 117.96(19) C22 C17 P1 . . 121.05(14) C18 C17 P1 . . 120.96(16) C19 C18 C17 . . 120.5(2) C19 C18 H18 . . 119.8 C17 C18 H18 . . 119.8 C20 C19 C18 . . 120.4(2) C20 C19 H19 . . 119.8 C18 C19 H19 . . 119.8 C21 C20 C19 . . 119.7(2) C21 C20 H20 . . 120.2 C19 C20 H20 . . 120.2 C20 C21 C22 . . 120.3(3) C20 C21 H21 . . 119.9 C22 C21 H21 . . 119.9 C17 C22 C21 . . 121.2(2) C17 C22 H22 . . 119.4 C21 C22 H22 . . 119.4 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Mo1 C1 . 2.034(2) Mo1 C1 2_557 2.034(2) Mo1 C2 2_557 2.035(2) Mo1 C2 . 2.035(2) Mo1 P1 2_557 2.4879(5) Mo1 P1 . 2.4879(5) P1 C5 . 1.8341(19) P1 C11 . 1.8430(19) P1 C17 . 1.8430(19) O1 C1 . 1.143(3) O2 C2 . 1.141(2) C5 C10 . 1.376(3) C5 C6 . 1.389(3) C6 C7 . 1.378(3) C6 H6 . 0.93 C7 C8 . 1.354(4) C7 H7 . 0.93 C8 C9 . 1.367(4) C8 H8 . 0.93 C9 C10 . 1.386(3) C9 H9 . 0.93 C10 H10 . 0.93 C11 C16 . 1.373(3) C11 C12 . 1.380(3) C12 C13 . 1.376(3) C12 H12 . 0.93 C13 C14 . 1.343(4) C13 H13 . 0.93 C14 C15 . 1.353(4) C14 H14 . 0.93 C15 C16 . 1.395(4) C15 H15 . 0.93 C16 H16 . 0.93 C17 C22 . 1.370(3) C17 C18 . 1.390(3) C18 C19 . 1.381(3) C18 H18 . 0.93 C19 C20 . 1.374(4) C19 H19 . 0.93 C20 C21 . 1.352(4) C20 H20 . 0.93 C21 C22 . 1.390(3) C21 H21 . 0.93 C22 H22 . 0.93