# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef 'Gesamtcif.cif' _audit_creation_method 'manual editing of form.cif' _publ_contact_author_phone '049 228 73-5345' _publ_contact_author_fax '049 228 73-9616' _publ_contact_author_email r.streubel@uni-bonn.de _publ_contact_author_name 'Streubel, Rainer' _publ_contact_author_address ; Institut f\"ur Anorganische Chemie Rheinische Friedrich-Wilhelms-University of Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Germany ; _publ_section_title ; First Examples of Oxaphosphirane Pentacarbonylchromium(0) and -molybdenum(0) Complexes: Synthesis, Structures and Reactions ; loop_ _publ_author_name _publ_author_address 'Albrecht, Carolin' ; Institut f\"ur Anorganische Chemie Rheinische Friedrich-Wilhelms-University of Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Germany ; 'Bode, Maren' ; Institut f\"ur Anorganische Chemie Rheinische Friedrich-Wilhelms-University of Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Germany ; 'Perez, Janaina Marinas' ; Institut f\"ur Anorganische Chemie Rheinische Friedrich-Wilhelms-University of Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Germany ; 'Daniels, J\"org' ; Institut f\"ur Anorganische Chemie Rheinische Friedrich-Wilhelms-University of Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Germany ; 'Schnakenburg, Gregor' ; Institut f\"ur Anorganische Chemie Rheinische Friedrich-Wilhelms-University of Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Germany ; 'Streubel, Rainer' ; Institut f\"ur Anorganische Chemie Rheinische Friedrich-Wilhelms-University of Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Germany ; #------------------------------------------------------------------------------ data_joerg01 _database_code_depnum_ccdc_archive 'CCDC 792183' #TrackingRef 'Gesamtcif.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H19 Cr O6 P' _chemical_formula_sum 'C17 H19 Cr O6 P' _chemical_formula_weight 402.29 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' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2548(4) _cell_length_b 13.4470(9) _cell_length_c 15.3120(9) _cell_angle_alpha 87.438(3) _cell_angle_beta 86.721(4) _cell_angle_gamma 88.908(4) _cell_volume 1900.29(19) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 15981 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 30.03 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.714 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.8306 _exptl_absorpt_correction_T_max 0.9720 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16880 _diffrn_reflns_av_R_equivalents 0.0799 _diffrn_reflns_av_sigmaI/netI 0.0962 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6658 _reflns_number_gt 4455 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6658 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1496 _refine_ls_wR_factor_gt 0.1370 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8271(4) 0.3095(3) 0.1598(3) 0.0279(10) Uani 1 1 d . . . H1A H 0.9141 0.2726 0.1809 0.034 Uiso 1 1 calc R . . C2 C 0.8054(5) 0.3036(4) 0.0644(3) 0.0362(12) Uani 1 1 d . . . H2C H 0.8937 0.3243 0.0306 0.054 Uiso 1 1 calc R . . H2B H 0.7246 0.3476 0.0484 0.054 Uiso 1 1 calc R . . H2A H 0.7835 0.2349 0.0515 0.054 Uiso 1 1 calc R . . C3 C 0.8697(4) 0.4037(3) 0.3240(3) 0.0227(10) Uani 1 1 d . . . C4 C 0.9895(4) 0.4806(3) 0.3080(3) 0.0255(10) Uani 1 1 d . . . C5 C 0.9661(4) 0.5532(3) 0.3640(3) 0.0263(10) Uani 1 1 d . . . C6 C 0.8328(4) 0.5357(3) 0.4187(3) 0.0236(10) Uani 1 1 d . . . C7 C 0.7760(4) 0.4486(3) 0.3972(3) 0.0224(10) Uani 1 1 d . . . C8 C 0.9245(5) 0.2996(3) 0.3488(3) 0.0317(11) Uani 1 1 d . . . H8A H 0.9645 0.2993 0.4067 0.047 Uiso 1 1 calc R . . H8B H 1.0001 0.2793 0.3054 0.047 Uiso 1 1 calc R . . H8C H 0.8442 0.2529 0.3502 0.047 Uiso 1 1 calc R . . C9 C 1.1111(4) 0.4674(4) 0.2393(3) 0.0385(13) Uani 1 1 d . . . H9A H 1.0710 0.4638 0.1817 0.058 Uiso 1 1 calc R . . H9B H 1.1652 0.4058 0.2529 0.058 Uiso 1 1 calc R . . H9C H 1.1762 0.5242 0.2388 0.058 Uiso 1 1 calc R . . C10 C 1.0591(5) 0.6429(4) 0.3748(3) 0.0379(12) Uani 1 1 d . . . H10A H 1.1384 0.6444 0.3296 0.057 Uiso 1 1 calc R . . H10B H 1.0990 0.6384 0.4328 0.057 Uiso 1 1 calc R . . H10C H 0.9999 0.7038 0.3690 0.057 Uiso 1 1 calc R . . C11 C 0.7752(5) 0.6037(4) 0.4885(3) 0.0351(12) Uani 1 1 d . . . H11A H 0.7672 0.6718 0.4635 0.053 Uiso 1 1 calc R . . H11B H 0.8413 0.6021 0.5363 0.053 Uiso 1 1 calc R . . H11C H 0.6795 0.5813 0.5111 0.053 Uiso 1 1 calc R . . C12 C 0.6484(4) 0.3935(3) 0.4382(3) 0.0284(10) Uani 1 1 d . . . H12A H 0.6820 0.3332 0.4696 0.043 Uiso 1 1 calc R . . H12B H 0.5853 0.3752 0.3924 0.043 Uiso 1 1 calc R . . H12C H 0.5943 0.4362 0.4792 0.043 Uiso 1 1 calc R . . C13 C 0.5218(5) 0.6517(4) 0.1214(3) 0.0308(11) Uani 1 1 d . . . C14 C 0.7705(4) 0.5567(3) 0.0741(3) 0.0266(10) Uani 1 1 d . . . C15 C 0.7365(4) 0.6509(4) 0.2274(3) 0.0267(10) Uani 1 1 d . . . C16 C 0.5097(5) 0.5468(3) 0.2751(3) 0.0299(11) Uani 1 1 d . . . C17 C 0.5135(4) 0.4608(4) 0.1210(3) 0.0288(11) Uani 1 1 d . . . C18 C 0.2931(5) 1.1770(4) 0.1399(3) 0.0342(11) Uani 1 1 d . . . H18A H 0.3721 1.2219 0.1549 0.041 Uiso 1 1 calc R . . C19 C 0.2630(5) 1.1779(4) 0.0455(3) 0.0437(13) Uani 1 1 d . . . H19C H 0.3531 1.1649 0.0107 0.066 Uiso 1 1 calc R . . H19B H 0.2230 1.2432 0.0274 0.066 Uiso 1 1 calc R . . H19A H 0.1930 1.1262 0.0360 0.066 Uiso 1 1 calc R . . C20 C 0.3601(4) 1.0937(3) 0.3140(3) 0.0219(10) Uani 1 1 d . . . C21 C 0.2704(4) 1.0498(3) 0.3909(3) 0.0221(10) Uani 1 1 d . . . C22 C 0.3366(4) 0.9686(3) 0.4230(3) 0.0241(10) Uani 1 1 d . . . C23 C 0.4766(4) 0.9513(3) 0.3718(3) 0.0282(11) Uani 1 1 d . . . C24 C 0.4915(4) 1.0237(3) 0.3081(3) 0.0259(10) Uani 1 1 d . . . C25 C 0.3999(5) 1.2031(3) 0.3250(3) 0.0310(11) Uani 1 1 d . . . H25A H 0.4387 1.2098 0.3827 0.047 Uiso 1 1 calc R . . H25B H 0.3132 1.2456 0.3202 0.047 Uiso 1 1 calc R . . H25C H 0.4730 1.2236 0.2792 0.047 Uiso 1 1 calc R . . C26 C 0.1335(4) 1.1010(3) 0.4256(3) 0.0276(10) Uani 1 1 d . . . H26A H 0.0627 1.1045 0.3803 0.041 Uiso 1 1 calc R . . H26B H 0.1557 1.1685 0.4418 0.041 Uiso 1 1 calc R . . H26C H 0.0932 1.0632 0.4773 0.041 Uiso 1 1 calc R . . C27 C 0.2859(5) 0.9003(4) 0.4985(3) 0.0353(12) Uani 1 1 d . . . H27A H 0.2550 0.8374 0.4763 0.053 Uiso 1 1 calc R . . H27B H 0.2044 0.9317 0.5311 0.053 Uiso 1 1 calc R . . H27C H 0.3654 0.8874 0.5373 0.053 Uiso 1 1 calc R . . C28 C 0.5794(5) 0.8692(4) 0.3947(3) 0.0363(12) Uani 1 1 d . . . H28A H 0.5305 0.8052 0.3938 0.054 Uiso 1 1 calc R . . H28B H 0.6129 0.8781 0.4534 0.054 Uiso 1 1 calc R . . H28C H 0.6625 0.8700 0.3521 0.054 Uiso 1 1 calc R . . C29 C 0.6146(4) 1.0391(4) 0.2413(3) 0.0389(13) Uani 1 1 d . . . H29C H 0.6834 0.9830 0.2456 0.058 Uiso 1 1 calc R . . H29B H 0.6637 1.1010 0.2520 0.058 Uiso 1 1 calc R . . H29A H 0.5774 1.0434 0.1826 0.058 Uiso 1 1 calc R . . C30 C 0.0775(5) 0.8068(4) 0.1462(3) 0.0417(13) Uani 1 1 d . . . C31 C 0.2877(4) 0.9256(3) 0.0782(3) 0.0280(10) Uani 1 1 d . . . C32 C 0.0141(5) 0.9963(4) 0.1244(3) 0.0375(12) Uani 1 1 d . . . C33 C 0.0395(4) 0.9201(3) 0.2848(3) 0.0290(11) Uani 1 1 d . . . C34 C 0.2931(5) 0.8382(4) 0.2394(3) 0.0291(11) Uani 1 1 d . . . Cr1 Cr 0.63521(6) 0.55029(5) 0.17306(4) 0.02111(19) Uani 1 1 d . . . Cr2 Cr 0.15995(7) 0.92292(5) 0.18119(4) 0.0234(2) Uani 1 1 d . . . O1 O 0.6938(3) 0.2997(2) 0.2184(2) 0.0284(7) Uani 1 1 d . . . O2 O 0.4523(3) 0.7116(3) 0.0888(2) 0.0427(9) Uani 1 1 d . . . O3 O 0.8524(3) 0.5624(2) 0.0155(2) 0.0384(8) Uani 1 1 d . . . O4 O 0.7864(3) 0.7167(3) 0.2593(2) 0.0386(8) Uani 1 1 d . . . O5 O 0.4325(3) 0.5483(3) 0.3371(2) 0.0394(9) Uani 1 1 d . . . O6 O 0.4342(3) 0.4093(3) 0.0900(2) 0.0403(9) Uani 1 1 d . . . O8 O 0.0274(4) 0.7341(3) 0.1250(3) 0.0659(13) Uani 1 1 d . . . O7 O 0.1608(3) 1.1780(2) 0.2005(2) 0.0318(8) Uani 1 1 d . . . O9 O 0.3651(3) 0.9266(2) 0.0176(2) 0.0342(8) Uani 1 1 d . . . O10 O -0.0782(3) 1.0384(3) 0.0908(2) 0.0534(11) Uani 1 1 d . . . O11 O -0.0364(3) 0.9151(3) 0.3476(2) 0.0408(9) Uani 1 1 d . . . O12 O 0.3625(4) 0.7781(3) 0.2734(2) 0.0435(9) Uani 1 1 d . . . P1 P 0.76624(11) 0.41173(8) 0.22401(7) 0.0211(3) Uani 1 1 d . . . P2 P 0.25822(11) 1.07405(9) 0.21575(8) 0.0230(3) Uani 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 C1 0.030(2) 0.017(3) 0.037(3) -0.005(2) 0.0021(19) 0.0013(18) C2 0.042(3) 0.027(3) 0.040(3) -0.014(2) 0.001(2) 0.001(2) C3 0.025(2) 0.014(2) 0.028(3) 0.001(2) -0.0002(17) 0.0034(17) C4 0.022(2) 0.028(3) 0.026(3) 0.002(2) -0.0038(17) 0.0019(18) C5 0.025(2) 0.026(3) 0.029(3) 0.007(2) -0.0113(18) -0.0054(18) C6 0.024(2) 0.017(2) 0.030(3) 0.000(2) -0.0055(18) 0.0031(17) C7 0.021(2) 0.024(3) 0.023(2) 0.001(2) -0.0043(16) 0.0031(17) C8 0.036(2) 0.021(3) 0.037(3) 0.001(2) -0.006(2) 0.0080(19) C9 0.021(2) 0.050(4) 0.044(3) -0.004(3) 0.003(2) -0.001(2) C10 0.029(2) 0.033(3) 0.052(3) 0.003(3) -0.008(2) -0.012(2) C11 0.030(2) 0.035(3) 0.041(3) -0.007(3) -0.003(2) -0.003(2) C12 0.027(2) 0.023(3) 0.035(3) 0.001(2) -0.0002(19) -0.0009(18) C13 0.031(2) 0.030(3) 0.031(3) -0.004(2) 0.000(2) 0.003(2) C14 0.029(2) 0.020(3) 0.032(3) 0.000(2) -0.006(2) 0.0023(18) C15 0.025(2) 0.022(3) 0.033(3) -0.003(2) -0.0026(18) 0.0079(19) C16 0.028(2) 0.025(3) 0.037(3) 0.000(2) -0.010(2) 0.0048(19) C17 0.028(2) 0.029(3) 0.029(3) 0.002(2) -0.0059(19) 0.006(2) C18 0.040(3) 0.024(3) 0.036(3) 0.005(2) 0.007(2) -0.001(2) C19 0.053(3) 0.031(3) 0.046(3) 0.008(3) 0.005(2) 0.007(2) C20 0.022(2) 0.015(2) 0.029(3) 0.000(2) -0.0009(17) 0.0009(16) C21 0.020(2) 0.019(2) 0.027(2) -0.003(2) -0.0007(17) -0.0007(17) C22 0.022(2) 0.023(3) 0.028(3) 0.000(2) -0.0059(17) 0.0006(18) C23 0.022(2) 0.027(3) 0.038(3) -0.012(2) -0.0113(18) 0.0015(18) C24 0.015(2) 0.026(3) 0.037(3) -0.002(2) -0.0008(17) -0.0006(17) C25 0.033(2) 0.019(3) 0.041(3) -0.002(2) 0.001(2) -0.0068(19) C26 0.025(2) 0.021(3) 0.036(3) 0.001(2) 0.0028(18) 0.0025(18) C27 0.035(3) 0.029(3) 0.041(3) 0.003(2) -0.001(2) 0.002(2) C28 0.027(2) 0.032(3) 0.050(3) -0.003(3) -0.013(2) 0.007(2) C29 0.022(2) 0.042(3) 0.052(3) 0.003(3) 0.007(2) 0.002(2) C30 0.040(3) 0.048(4) 0.037(3) -0.009(3) 0.011(2) -0.016(2) C31 0.026(2) 0.022(3) 0.036(3) -0.006(2) -0.005(2) 0.0016(18) C32 0.029(3) 0.050(4) 0.033(3) -0.003(3) 0.006(2) -0.005(2) C33 0.026(2) 0.027(3) 0.035(3) -0.004(2) -0.003(2) -0.0063(19) C34 0.039(3) 0.020(3) 0.028(3) -0.004(2) 0.001(2) -0.004(2) Cr1 0.0192(3) 0.0186(4) 0.0254(4) -0.0002(3) -0.0012(3) 0.0028(3) Cr2 0.0230(4) 0.0225(4) 0.0246(4) -0.0011(3) 0.0007(3) -0.0039(3) O1 0.0274(15) 0.0226(18) 0.0353(18) -0.0010(15) -0.0013(13) -0.0050(12) O2 0.0470(19) 0.039(2) 0.041(2) 0.0050(18) -0.0077(16) 0.0194(17) O3 0.0362(18) 0.036(2) 0.041(2) 0.0023(17) 0.0073(16) 0.0019(15) O4 0.0404(19) 0.029(2) 0.048(2) -0.0106(18) -0.0073(15) -0.0016(15) O5 0.0355(18) 0.047(2) 0.033(2) 0.0026(17) 0.0079(15) 0.0135(15) O6 0.0363(19) 0.036(2) 0.050(2) -0.0106(18) -0.0100(15) -0.0044(16) O8 0.082(3) 0.063(3) 0.053(3) -0.024(2) 0.024(2) -0.045(2) O7 0.0312(16) 0.0260(19) 0.0371(19) 0.0017(16) 0.0007(13) 0.0111(13) O9 0.0348(17) 0.032(2) 0.035(2) 0.0005(16) 0.0062(15) 0.0018(14) O10 0.0337(19) 0.078(3) 0.048(2) 0.004(2) -0.0073(17) 0.0118(19) O11 0.0380(18) 0.047(2) 0.037(2) -0.0076(18) 0.0087(16) -0.0134(16) O12 0.061(2) 0.023(2) 0.048(2) -0.0018(18) -0.0147(18) 0.0048(17) P1 0.0192(5) 0.0179(6) 0.0262(7) -0.0007(5) 0.0000(4) 0.0000(4) P2 0.0220(6) 0.0190(6) 0.0274(7) 0.0021(5) 0.0013(4) 0.0017(4) _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. ; 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 C1 O1 1.488(5) . ? C1 C2 1.492(6) . ? C1 P1 1.789(4) . ? C1 H1A 1.0000 . ? C2 H2C 0.9800 . ? C2 H2B 0.9800 . ? C2 H2A 0.9800 . ? C3 C7 1.517(6) . ? C3 C8 1.520(6) . ? C3 C4 1.532(6) . ? C3 P1 1.850(4) . ? C4 C5 1.335(6) . ? C4 C9 1.509(6) . ? C5 C6 1.467(6) . ? C5 C10 1.516(6) . ? C6 C7 1.354(6) . ? C6 C11 1.506(6) . ? C7 C12 1.497(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 O2 1.136(5) . ? C13 Cr1 1.880(5) . ? C14 O3 1.142(5) . ? C14 Cr1 1.909(5) . ? C15 O4 1.146(5) . ? C15 Cr1 1.908(5) . ? C16 O5 1.156(5) . ? C16 Cr1 1.892(5) . ? C17 O6 1.154(5) . ? C17 Cr1 1.895(5) . ? C18 C19 1.487(7) . ? C18 O7 1.494(5) . ? C18 P2 1.789(5) . ? C18 H18A 1.0000 . ? C19 H19C 0.9800 . ? C19 H19B 0.9800 . ? C19 H19A 0.9800 . ? C20 C21 1.506(5) . ? C20 C24 1.525(6) . ? C20 C25 1.543(6) . ? C20 P2 1.852(4) . ? C21 C22 1.331(6) . ? C21 C26 1.511(5) . ? C22 C23 1.495(6) . ? C22 C27 1.503(6) . ? C23 C24 1.350(6) . ? C23 C28 1.487(6) . ? C24 C29 1.498(6) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29C 0.9800 . ? C29 H29B 0.9800 . ? C29 H29A 0.9800 . ? C30 O8 1.158(6) . ? C30 Cr2 1.864(5) . ? C31 O9 1.140(5) . ? C31 Cr2 1.915(5) . ? C32 O10 1.149(6) . ? C32 Cr2 1.887(5) . ? C33 O11 1.158(5) . ? C33 Cr2 1.886(5) . ? C34 O12 1.148(5) . ? C34 Cr2 1.896(5) . ? Cr1 P1 2.3331(13) . ? Cr2 P2 2.3363(13) . ? O1 P1 1.668(3) . ? O7 P2 1.664(3) . ? 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 O1 C1 C2 115.4(3) . . ? O1 C1 P1 60.38(19) . . ? C2 C1 P1 124.0(4) . . ? O1 C1 H1A 115.1 . . ? C2 C1 H1A 115.1 . . ? P1 C1 H1A 115.1 . . ? C1 C2 H2C 109.5 . . ? C1 C2 H2B 109.5 . . ? H2C C2 H2B 109.5 . . ? C1 C2 H2A 109.5 . . ? H2C C2 H2A 109.5 . . ? H2B C2 H2A 109.5 . . ? C7 C3 C8 112.4(4) . . ? C7 C3 C4 102.2(3) . . ? C8 C3 C4 114.0(3) . . ? C7 C3 P1 107.7(3) . . ? C8 C3 P1 114.3(3) . . ? C4 C3 P1 105.2(3) . . ? C5 C4 C9 129.5(4) . . ? C5 C4 C3 108.8(4) . . ? C9 C4 C3 121.7(4) . . ? C4 C5 C6 110.7(4) . . ? C4 C5 C10 127.7(4) . . ? C6 C5 C10 121.6(4) . . ? C7 C6 C5 108.7(4) . . ? C7 C6 C11 127.1(4) . . ? C5 C6 C11 124.2(4) . . ? C6 C7 C12 129.8(4) . . ? C6 C7 C3 109.6(3) . . ? C12 C7 C3 120.5(4) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C13 Cr1 178.4(4) . . ? O3 C14 Cr1 178.6(4) . . ? O4 C15 Cr1 173.8(4) . . ? O5 C16 Cr1 177.6(4) . . ? O6 C17 Cr1 176.9(4) . . ? C19 C18 O7 114.3(4) . . ? C19 C18 P2 124.3(4) . . ? O7 C18 P2 60.1(2) . . ? C19 C18 H18A 115.3 . . ? O7 C18 H18A 115.3 . . ? P2 C18 H18A 115.3 . . ? C18 C19 H19C 109.5 . . ? C18 C19 H19B 109.5 . . ? H19C C19 H19B 109.5 . . ? C18 C19 H19A 109.5 . . ? H19C C19 H19A 109.5 . . ? H19B C19 H19A 109.5 . . ? C21 C20 C24 103.1(3) . . ? C21 C20 C25 113.1(4) . . ? C24 C20 C25 113.2(3) . . ? C21 C20 P2 106.3(3) . . ? C24 C20 P2 106.2(3) . . ? C25 C20 P2 114.0(3) . . ? C22 C21 C20 109.6(4) . . ? C22 C21 C26 128.8(4) . . ? C20 C21 C26 121.4(4) . . ? C21 C22 C23 109.9(4) . . ? C21 C22 C27 128.0(4) . . ? C23 C22 C27 122.1(4) . . ? C24 C23 C28 128.8(4) . . ? C24 C23 C22 108.4(4) . . ? C28 C23 C22 122.7(4) . . ? C23 C24 C29 128.3(4) . . ? C23 C24 C20 109.1(4) . . ? C29 C24 C20 122.7(4) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29C 109.5 . . ? C24 C29 H29B 109.5 . . ? H29C C29 H29B 109.5 . . ? C24 C29 H29A 109.5 . . ? H29C C29 H29A 109.5 . . ? H29B C29 H29A 109.5 . . ? O8 C30 Cr2 179.2(6) . . ? O9 C31 Cr2 179.1(4) . . ? O10 C32 Cr2 177.6(5) . . ? O11 C33 Cr2 177.5(4) . . ? O12 C34 Cr2 171.9(4) . . ? C13 Cr1 C16 90.88(19) . . ? C13 Cr1 C17 85.84(19) . . ? C16 Cr1 C17 89.72(19) . . ? C13 Cr1 C15 88.2(2) . . ? C16 Cr1 C15 86.21(19) . . ? C17 Cr1 C15 172.77(18) . . ? C13 Cr1 C14 90.46(19) . . ? C16 Cr1 C14 176.63(18) . . ? C17 Cr1 C14 93.46(19) . . ? C15 Cr1 C14 90.74(18) . . ? C13 Cr1 P1 172.90(15) . . ? C16 Cr1 P1 91.78(14) . . ? C17 Cr1 P1 87.59(14) . . ? C15 Cr1 P1 98.50(14) . . ? C14 Cr1 P1 87.25(14) . . ? C30 Cr2 C33 90.82(19) . . ? C30 Cr2 C32 88.4(2) . . ? C33 Cr2 C32 88.9(2) . . ? C30 Cr2 C34 86.3(2) . . ? C33 Cr2 C34 88.71(19) . . ? C32 Cr2 C34 174.1(2) . . ? C30 Cr2 C31 90.14(19) . . ? C33 Cr2 C31 178.13(18) . . ? C32 Cr2 C31 92.77(19) . . ? C34 Cr2 C31 89.74(19) . . ? C30 Cr2 P2 175.92(18) . . ? C33 Cr2 P2 91.35(14) . . ? C32 Cr2 P2 88.19(16) . . ? C34 Cr2 P2 97.23(14) . . ? C31 Cr2 P2 87.80(13) . . ? C1 O1 P1 68.8(2) . . ? C18 O7 P2 68.8(2) . . ? O1 P1 C1 50.84(16) . . ? O1 P1 C3 105.10(17) . . ? C1 P1 C3 106.5(2) . . ? O1 P1 Cr1 118.11(11) . . ? C1 P1 Cr1 125.37(16) . . ? C3 P1 Cr1 126.01(14) . . ? O7 P2 C18 51.10(18) . . ? O7 P2 C20 105.27(18) . . ? C18 P2 C20 107.7(2) . . ? O7 P2 Cr2 118.57(12) . . ? C18 P2 Cr2 125.13(17) . . ? C20 P2 Cr2 124.98(14) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.655 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.095 #------------------------------------------------------------------------------ data_Greg283 _database_code_depnum_ccdc_archive 'CCDC 792184' #TrackingRef 'Gesamtcif.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H19 Mo O6 P' _chemical_formula_sum 'C17 H19 Mo O6 P' _chemical_formula_weight 446.23 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' Mo Mo -1.6832 0.6857 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3112(3) _cell_length_b 13.6564(3) _cell_length_c 15.4475(3) _cell_angle_alpha 87.2385(15) _cell_angle_beta 86.4875(15) _cell_angle_gamma 89.1165(13) _cell_volume 1958.15(9) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 20869 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 34.975 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.779 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.77032 _exptl_absorpt_correction_T_max 0.88763 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29432 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 30.50 _reflns_number_total 11948 _reflns_number_gt 9034 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0126P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11948 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0587 _refine_ls_wR_factor_gt 0.0548 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8363(2) 0.30325(12) 0.16657(10) 0.0226(4) Uani 1 1 d . . . H1A H 0.9222 0.2671 0.1882 0.027 Uiso 1 1 calc R . . C2 C 0.8154(2) 0.29639(13) 0.07143(10) 0.0310(5) Uani 1 1 d . . . H2C H 0.9045 0.3147 0.0379 0.046 Uiso 1 1 calc R . . H2B H 0.7374 0.3410 0.0547 0.046 Uiso 1 1 calc R . . H2A H 0.7907 0.2290 0.0596 0.046 Uiso 1 1 calc R . . C3 C 0.87689(19) 0.40042(11) 0.32785(9) 0.0175(3) Uani 1 1 d . . . C4 C 0.99562(19) 0.47531(12) 0.31057(10) 0.0202(4) Uani 1 1 d . . . C5 C 0.9687(2) 0.54984(12) 0.36396(10) 0.0210(4) Uani 1 1 d . . . C6 C 0.8355(2) 0.53136(11) 0.41714(9) 0.0190(4) Uani 1 1 d . . . C7 C 0.78024(19) 0.44492(11) 0.39804(9) 0.0172(3) Uani 1 1 d . . . C8 C 0.9312(2) 0.29744(12) 0.35430(10) 0.0251(4) Uani 1 1 d . . . H8A H 0.9680 0.2978 0.4124 0.038 Uiso 1 1 calc R . . H8B H 1.0085 0.2776 0.3126 0.038 Uiso 1 1 calc R . . H8C H 0.8519 0.2510 0.3549 0.038 Uiso 1 1 calc R . . C9 C 1.1188(2) 0.46132(14) 0.24483(11) 0.0331(5) Uani 1 1 d . . . H9A H 1.0814 0.4491 0.1885 0.050 Uiso 1 1 calc R . . H9B H 1.1781 0.4052 0.2636 0.050 Uiso 1 1 calc R . . H9C H 1.1775 0.5205 0.2395 0.050 Uiso 1 1 calc R . . C10 C 1.0611(2) 0.63792(13) 0.37217(12) 0.0310(4) Uani 1 1 d . . . H10A H 1.1356 0.6410 0.3245 0.046 Uiso 1 1 calc R . . H10B H 1.1066 0.6326 0.4278 0.046 Uiso 1 1 calc R . . H10C H 1.0012 0.6975 0.3696 0.046 Uiso 1 1 calc R . . C11 C 0.7747(2) 0.60083(13) 0.48336(10) 0.0298(4) Uani 1 1 d . . . H11A H 0.7641 0.6664 0.4557 0.045 Uiso 1 1 calc R . . H11B H 0.8400 0.6035 0.5306 0.045 Uiso 1 1 calc R . . H11C H 0.6804 0.5777 0.5068 0.045 Uiso 1 1 calc R . . C12 C 0.6517(2) 0.39220(12) 0.43844(10) 0.0246(4) Uani 1 1 d . . . H12A H 0.6834 0.3351 0.4735 0.037 Uiso 1 1 calc R . . H12B H 0.5927 0.3706 0.3927 0.037 Uiso 1 1 calc R . . H12C H 0.5949 0.4364 0.4756 0.037 Uiso 1 1 calc R . . C13 C 0.5135(2) 0.65212(13) 0.11695(10) 0.0248(4) Uani 1 1 d . . . C14 C 0.7788(2) 0.55511(12) 0.06457(10) 0.0225(4) Uani 1 1 d . . . C15 C 0.7443(2) 0.65622(13) 0.22888(10) 0.0237(4) Uani 1 1 d . . . C16 C 0.5029(2) 0.54567(12) 0.28199(10) 0.0231(4) Uani 1 1 d . . . C17 C 0.5088(2) 0.44975(13) 0.11975(10) 0.0238(4) Uani 1 1 d . . . C18 C 0.2936(2) 1.17626(12) 0.14350(10) 0.0266(4) Uani 1 1 d . . . H18A H 0.3712 1.2214 0.1580 0.032 Uiso 1 1 calc R . . C19 C 0.2639(2) 1.17653(14) 0.04910(11) 0.0360(5) Uani 1 1 d . . . H19C H 0.3539 1.1650 0.0146 0.054 Uiso 1 1 calc R . . H19B H 0.2225 1.2402 0.0311 0.054 Uiso 1 1 calc R . . H19A H 0.1957 1.1245 0.0400 0.054 Uiso 1 1 calc R . . C20 C 0.36479(19) 1.09323(11) 0.31577(9) 0.0188(4) Uani 1 1 d . . . C21 C 0.27238(19) 1.04929(11) 0.39110(9) 0.0173(3) Uani 1 1 d . . . C22 C 0.3385(2) 0.96765(11) 0.42259(10) 0.0191(4) Uani 1 1 d . . . C23 C 0.4772(2) 0.95347(12) 0.37348(10) 0.0210(4) Uani 1 1 d . . . C24 C 0.49435(19) 1.02483(12) 0.31039(10) 0.0209(4) Uani 1 1 d . . . C25 C 0.4020(2) 1.20104(12) 0.32759(11) 0.0272(4) Uani 1 1 d . . . H25A H 0.4387 1.2074 0.3851 0.041 Uiso 1 1 calc R . . H25B H 0.3153 1.2420 0.3223 0.041 Uiso 1 1 calc R . . H25C H 0.4755 1.2224 0.2828 0.041 Uiso 1 1 calc R . . C26 C 0.1355(2) 1.09652(12) 0.42357(10) 0.0228(4) Uani 1 1 d . . . H26A H 0.0687 1.1019 0.3769 0.034 Uiso 1 1 calc R . . H26B H 0.1554 1.1621 0.4426 0.034 Uiso 1 1 calc R . . H26C H 0.0923 1.0567 0.4726 0.034 Uiso 1 1 calc R . . C27 C 0.2851(2) 0.89932(12) 0.49645(10) 0.0285(4) Uani 1 1 d . . . H27A H 0.2648 0.8353 0.4742 0.043 Uiso 1 1 calc R . . H27B H 0.1970 0.9266 0.5243 0.043 Uiso 1 1 calc R . . H27C H 0.3588 0.8915 0.5390 0.043 Uiso 1 1 calc R . . C28 C 0.5816(2) 0.87239(13) 0.39636(12) 0.0316(5) Uani 1 1 d . . . H28A H 0.5306 0.8101 0.4038 0.047 Uiso 1 1 calc R . . H28B H 0.6251 0.8863 0.4506 0.047 Uiso 1 1 calc R . . H28C H 0.6572 0.8680 0.3496 0.047 Uiso 1 1 calc R . . C29 C 0.6188(2) 1.04113(14) 0.24553(12) 0.0337(5) Uani 1 1 d . . . H29C H 0.6896 0.9879 0.2524 0.051 Uiso 1 1 calc R . . H29B H 0.6636 1.1039 0.2550 0.051 Uiso 1 1 calc R . . H29A H 0.5847 1.0423 0.1867 0.051 Uiso 1 1 calc R . . C30 C 0.0813(2) 0.78969(15) 0.14510(11) 0.0349(5) Uani 1 1 d . . . C31 C 0.2981(2) 0.92164(12) 0.07020(10) 0.0219(4) Uani 1 1 d . . . C32 C 0.0038(2) 0.99162(15) 0.12214(11) 0.0315(5) Uani 1 1 d . . . C33 C 0.0357(2) 0.90937(12) 0.29363(11) 0.0253(4) Uani 1 1 d . . . C34 C 0.3109(2) 0.82799(13) 0.24271(11) 0.0275(4) Uani 1 1 d . . . Mo1 Mo 0.636466(16) 0.548051(10) 0.172260(8) 0.01593(4) Uani 1 1 d . . . Mo2 Mo 0.163975(17) 0.915165(10) 0.181392(8) 0.01839(4) Uani 1 1 d . . . O1 O 0.70275(14) 0.29460(8) 0.22416(7) 0.0227(3) Uani 1 1 d . . . O2 O 0.44194(16) 0.70935(9) 0.08336(8) 0.0377(4) Uani 1 1 d . . . O3 O 0.85739(16) 0.56049(9) 0.00552(8) 0.0348(3) Uani 1 1 d . . . O4 O 0.79088(15) 0.72131(9) 0.26004(8) 0.0334(3) Uani 1 1 d . . . O5 O 0.42899(16) 0.54784(10) 0.34354(8) 0.0366(3) Uani 1 1 d . . . O6 O 0.43128(16) 0.39758(9) 0.09143(8) 0.0361(3) Uani 1 1 d . . . O8 O 0.03627(19) 0.71706(11) 0.12501(9) 0.0581(5) Uani 1 1 d . . . O7 O 0.16347(14) 1.17523(8) 0.20439(7) 0.0266(3) Uani 1 1 d . . . O9 O 0.37246(15) 0.92458(9) 0.00894(7) 0.0301(3) Uani 1 1 d . . . O10 O -0.08802(17) 1.03272(12) 0.09038(9) 0.0496(4) Uani 1 1 d . . . O11 O -0.03694(16) 0.90444(10) 0.35580(8) 0.0377(4) Uani 1 1 d . . . O12 O 0.38404(17) 0.77126(9) 0.27502(8) 0.0414(4) Uani 1 1 d . . . P1 P 0.77606(5) 0.40518(3) 0.22792(2) 0.01642(9) Uani 1 1 d . . . P2 P 0.26376(5) 1.07362(3) 0.21804(3) 0.01814(9) Uani 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 C1 0.0224(11) 0.0220(9) 0.0237(8) -0.0054(7) -0.0004(7) 0.0026(8) C2 0.0388(14) 0.0318(10) 0.0232(9) -0.0114(7) -0.0025(8) 0.0029(9) C3 0.0185(10) 0.0174(8) 0.0167(7) -0.0009(6) -0.0025(6) 0.0026(7) C4 0.0143(10) 0.0271(9) 0.0191(8) 0.0023(6) -0.0024(7) 0.0002(7) C5 0.0194(10) 0.0223(9) 0.0217(8) 0.0021(6) -0.0070(7) -0.0012(7) C6 0.0216(11) 0.0195(8) 0.0159(7) -0.0002(6) -0.0026(7) 0.0022(7) C7 0.0166(10) 0.0215(8) 0.0131(7) 0.0016(6) -0.0010(6) 0.0025(7) C8 0.0307(12) 0.0229(9) 0.0219(8) -0.0004(7) -0.0053(8) 0.0089(8) C9 0.0217(12) 0.0435(12) 0.0337(10) -0.0041(8) 0.0023(8) -0.0007(9) C10 0.0274(12) 0.0297(10) 0.0365(10) 0.0003(8) -0.0064(9) -0.0076(9) C11 0.0348(13) 0.0278(10) 0.0272(9) -0.0095(7) 0.0006(8) 0.0001(9) C12 0.0255(11) 0.0257(9) 0.0221(8) 0.0006(7) 0.0013(7) -0.0019(8) C13 0.0274(12) 0.0279(10) 0.0188(8) -0.0027(7) -0.0001(7) 0.0060(8) C14 0.0254(11) 0.0210(9) 0.0211(8) 0.0018(6) -0.0040(8) 0.0026(8) C15 0.0225(11) 0.0253(9) 0.0229(8) 0.0005(7) -0.0004(7) 0.0044(8) C16 0.0217(11) 0.0258(9) 0.0219(9) 0.0006(7) -0.0041(7) 0.0044(8) C17 0.0248(11) 0.0277(10) 0.0187(8) 0.0001(7) -0.0017(7) 0.0046(8) C18 0.0308(12) 0.0220(9) 0.0256(9) 0.0066(7) 0.0037(8) 0.0004(8) C19 0.0485(16) 0.0314(11) 0.0262(10) 0.0104(8) 0.0027(9) 0.0043(10) C20 0.0183(10) 0.0180(8) 0.0201(8) -0.0006(6) -0.0010(7) -0.0019(7) C21 0.0164(10) 0.0175(8) 0.0181(8) -0.0031(6) -0.0013(6) -0.0015(7) C22 0.0205(10) 0.0172(8) 0.0200(8) -0.0014(6) -0.0043(7) -0.0008(7) C23 0.0181(10) 0.0211(9) 0.0248(8) -0.0056(7) -0.0070(7) 0.0029(7) C24 0.0148(10) 0.0232(9) 0.0252(8) -0.0058(7) -0.0013(7) -0.0012(7) C25 0.0276(12) 0.0211(9) 0.0330(9) -0.0018(7) -0.0014(8) -0.0061(8) C26 0.0223(11) 0.0234(9) 0.0222(8) -0.0010(7) 0.0016(7) 0.0034(8) C27 0.0305(13) 0.0264(10) 0.0279(9) 0.0064(7) -0.0034(8) 0.0027(9) C28 0.0289(13) 0.0295(10) 0.0375(10) -0.0060(8) -0.0105(9) 0.0095(9) C29 0.0208(12) 0.0404(12) 0.0390(11) -0.0026(9) 0.0056(9) 0.0003(9) C30 0.0417(14) 0.0452(12) 0.0176(9) -0.0091(8) 0.0101(8) -0.0137(10) C31 0.0228(11) 0.0205(9) 0.0225(9) -0.0004(6) -0.0036(7) 0.0006(8) C32 0.0235(12) 0.0515(13) 0.0193(9) -0.0025(8) 0.0019(8) -0.0014(10) C33 0.0284(12) 0.0253(9) 0.0228(9) -0.0036(7) -0.0022(8) -0.0066(8) C34 0.0392(13) 0.0206(9) 0.0233(9) -0.0056(7) -0.0032(8) -0.0012(9) Mo1 0.01651(9) 0.01663(7) 0.01459(7) 0.00000(5) -0.00179(5) 0.00232(6) Mo2 0.01972(9) 0.02105(8) 0.01439(7) -0.00112(5) -0.00020(6) -0.00272(6) O1 0.0244(8) 0.0179(6) 0.0256(6) -0.0007(5) 0.0008(5) -0.0042(5) O2 0.0426(10) 0.0387(8) 0.0313(7) 0.0016(6) -0.0060(7) 0.0197(7) O3 0.0318(9) 0.0412(8) 0.0295(7) 0.0037(6) 0.0079(6) 0.0030(7) O4 0.0340(9) 0.0271(7) 0.0404(7) -0.0097(6) -0.0056(6) -0.0024(6) O5 0.0311(9) 0.0501(9) 0.0267(7) 0.0035(6) 0.0075(6) 0.0106(7) O6 0.0344(10) 0.0370(8) 0.0387(7) -0.0047(6) -0.0118(7) -0.0082(7) O8 0.0760(14) 0.0607(11) 0.0384(8) -0.0264(7) 0.0207(8) -0.0428(10) O7 0.0297(8) 0.0226(6) 0.0265(6) 0.0021(5) 0.0013(6) 0.0090(6) O9 0.0292(9) 0.0336(7) 0.0266(7) -0.0006(5) 0.0049(6) 0.0006(6) O10 0.0308(10) 0.0814(12) 0.0360(8) 0.0043(7) -0.0072(7) 0.0162(9) O11 0.0401(10) 0.0450(9) 0.0275(7) -0.0080(6) 0.0110(6) -0.0139(7) O12 0.0619(12) 0.0254(7) 0.0391(8) -0.0052(6) -0.0203(8) 0.0100(7) P1 0.0168(3) 0.0168(2) 0.01562(19) -0.00091(15) -0.00083(16) 0.00073(18) P2 0.0182(3) 0.0179(2) 0.0177(2) 0.00162(15) 0.00105(17) 0.00202(18) _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. ; 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 C1 O1 1.487(2) . ? C1 C2 1.502(2) . ? C1 P1 1.7856(16) . ? C1 H1A 1.0000 . ? C2 H2C 0.9800 . ? C2 H2B 0.9800 . ? C2 H2A 0.9800 . ? C3 C7 1.511(2) . ? C3 C4 1.520(2) . ? C3 C8 1.533(2) . ? C3 P1 1.8534(15) . ? C4 C5 1.352(2) . ? C4 C9 1.501(2) . ? C5 C6 1.463(2) . ? C5 C10 1.504(2) . ? C6 C7 1.348(2) . ? C6 C11 1.508(2) . ? C7 C12 1.494(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 O2 1.145(2) . ? C13 Mo1 2.0032(18) . ? C14 O3 1.134(2) . ? C14 Mo1 2.0621(18) . ? C15 O4 1.1352(19) . ? C15 Mo1 2.0574(18) . ? C16 O5 1.140(2) . ? C16 Mo1 2.0392(18) . ? C17 O6 1.142(2) . ? C17 Mo1 2.0359(18) . ? C18 O7 1.487(2) . ? C18 C19 1.501(2) . ? C18 P2 1.7847(17) . ? C18 H18A 1.0000 . ? C19 H19C 0.9800 . ? C19 H19B 0.9800 . ? C19 H19A 0.9800 . ? C20 C21 1.510(2) . ? C20 C24 1.515(2) . ? C20 C25 1.540(2) . ? C20 P2 1.8592(15) . ? C21 C22 1.350(2) . ? C21 C26 1.490(2) . ? C22 C23 1.472(2) . ? C22 C27 1.504(2) . ? C23 C24 1.349(2) . ? C23 C28 1.506(2) . ? C24 C29 1.497(2) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29C 0.9800 . ? C29 H29B 0.9800 . ? C29 H29A 0.9800 . ? C30 O8 1.146(2) . ? C30 Mo2 2.0073(19) . ? C31 O9 1.137(2) . ? C31 Mo2 2.0601(18) . ? C32 O10 1.139(2) . ? C32 Mo2 2.044(2) . ? C33 O11 1.140(2) . ? C33 Mo2 2.0433(18) . ? C34 O12 1.141(2) . ? C34 Mo2 2.046(2) . ? Mo1 P1 2.4763(5) . ? Mo2 P2 2.4720(4) . ? O1 P1 1.6719(11) . ? O7 P2 1.6727(12) . ? 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 O1 C1 C2 115.07(15) . . ? O1 C1 P1 60.63(7) . . ? C2 C1 P1 123.52(13) . . ? O1 C1 H1A 115.3 . . ? C2 C1 H1A 115.3 . . ? P1 C1 H1A 115.3 . . ? C1 C2 H2C 109.5 . . ? C1 C2 H2B 109.5 . . ? H2C C2 H2B 109.5 . . ? C1 C2 H2A 109.5 . . ? H2C C2 H2A 109.5 . . ? H2B C2 H2A 109.5 . . ? C7 C3 C4 103.41(13) . . ? C7 C3 C8 112.69(13) . . ? C4 C3 C8 113.96(15) . . ? C7 C3 P1 106.99(11) . . ? C4 C3 P1 105.20(10) . . ? C8 C3 P1 113.71(10) . . ? C5 C4 C9 129.29(16) . . ? C5 C4 C3 108.28(15) . . ? C9 C4 C3 122.42(14) . . ? C4 C5 C6 109.74(15) . . ? C4 C5 C10 126.80(17) . . ? C6 C5 C10 123.42(15) . . ? C7 C6 C5 109.93(14) . . ? C7 C6 C11 126.91(16) . . ? C5 C6 C11 123.16(15) . . ? C6 C7 C12 129.71(15) . . ? C6 C7 C3 108.63(15) . . ? C12 C7 C3 121.57(14) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C13 Mo1 177.66(15) . . ? O3 C14 Mo1 178.94(15) . . ? O4 C15 Mo1 172.93(16) . . ? O5 C16 Mo1 177.54(15) . . ? O6 C17 Mo1 176.50(16) . . ? O7 C18 C19 114.99(16) . . ? O7 C18 P2 60.69(8) . . ? C19 C18 P2 124.00(13) . . ? O7 C18 H18A 115.2 . . ? C19 C18 H18A 115.2 . . ? P2 C18 H18A 115.2 . . ? C18 C19 H19C 109.5 . . ? C18 C19 H19B 109.5 . . ? H19C C19 H19B 109.5 . . ? C18 C19 H19A 109.5 . . ? H19C C19 H19A 109.5 . . ? H19B C19 H19A 109.5 . . ? C21 C20 C24 103.46(13) . . ? C21 C20 C25 112.76(13) . . ? C24 C20 C25 114.11(15) . . ? C21 C20 P2 105.13(11) . . ? C24 C20 P2 106.26(10) . . ? C25 C20 P2 114.13(11) . . ? C22 C21 C26 128.90(15) . . ? C22 C21 C20 108.77(15) . . ? C26 C21 C20 122.26(14) . . ? C21 C22 C23 109.53(15) . . ? C21 C22 C27 127.43(17) . . ? C23 C22 C27 123.04(16) . . ? C24 C23 C22 109.56(16) . . ? C24 C23 C28 127.70(18) . . ? C22 C23 C28 122.69(15) . . ? C23 C24 C29 128.61(17) . . ? C23 C24 C20 108.65(15) . . ? C29 C24 C20 122.70(15) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29C 109.5 . . ? C24 C29 H29B 109.5 . . ? H29C C29 H29B 109.5 . . ? C24 C29 H29A 109.5 . . ? H29C C29 H29A 109.5 . . ? H29B C29 H29A 109.5 . . ? O8 C30 Mo2 178.7(2) . . ? O9 C31 Mo2 179.53(16) . . ? O10 C32 Mo2 178.21(19) . . ? O11 C33 Mo2 178.65(15) . . ? O12 C34 Mo2 172.79(16) . . ? C13 Mo1 C17 86.31(7) . . ? C13 Mo1 C16 90.48(7) . . ? C17 Mo1 C16 89.95(7) . . ? C13 Mo1 C15 88.83(7) . . ? C17 Mo1 C15 173.46(7) . . ? C16 Mo1 C15 85.71(7) . . ? C13 Mo1 C14 90.03(7) . . ? C17 Mo1 C14 93.09(7) . . ? C16 Mo1 C14 176.94(7) . . ? C15 Mo1 C14 91.29(7) . . ? C13 Mo1 P1 172.80(5) . . ? C17 Mo1 P1 86.83(5) . . ? C16 Mo1 P1 91.70(5) . . ? C15 Mo1 P1 98.17(5) . . ? C14 Mo1 P1 88.15(5) . . ? C30 Mo2 C33 90.93(7) . . ? C30 Mo2 C32 89.43(8) . . ? C33 Mo2 C32 88.71(7) . . ? C30 Mo2 C34 85.85(8) . . ? C33 Mo2 C34 88.68(7) . . ? C32 Mo2 C34 174.58(7) . . ? C30 Mo2 C31 90.09(7) . . ? C33 Mo2 C31 178.43(7) . . ? C32 Mo2 C31 92.50(7) . . ? C34 Mo2 C31 90.19(7) . . ? C30 Mo2 P2 176.87(5) . . ? C33 Mo2 P2 91.18(5) . . ? C32 Mo2 P2 88.30(6) . . ? C34 Mo2 P2 96.51(5) . . ? C31 Mo2 P2 87.85(5) . . ? C1 O1 P1 68.56(8) . . ? C18 O7 P2 68.49(8) . . ? O1 P1 C1 50.81(7) . . ? O1 P1 C3 105.60(6) . . ? C1 P1 C3 107.01(8) . . ? O1 P1 Mo1 117.35(5) . . ? C1 P1 Mo1 125.56(6) . . ? C3 P1 Mo1 125.57(5) . . ? O7 P2 C18 50.83(7) . . ? O7 P2 C20 105.09(7) . . ? C18 P2 C20 108.16(8) . . ? O7 P2 Mo2 118.54(5) . . ? C18 P2 Mo2 125.01(6) . . ? C20 P2 Mo2 124.86(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.556 _refine_diff_density_min -0.792 _refine_diff_density_rms 0.088 #------------------------------------------------------------------------------ data_khetestf _database_code_depnum_ccdc_archive 'CCDC 792185' #TrackingRef 'Gesamtcif.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H23 Cr O6 P' _chemical_formula_sum 'C19 H23 Cr O6 P' _chemical_formula_weight 430.34 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6335(4) _cell_length_b 10.2535(5) _cell_length_c 11.9380(6) _cell_angle_alpha 94.290(2) _cell_angle_beta 96.136(2) _cell_angle_gamma 90.618(2) _cell_volume 1047.61(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9817 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 35.00 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 0.653 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.7822 _exptl_absorpt_correction_T_max 0.8644 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8-KappaApexII' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35373 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0136 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5049 _reflns_number_gt 4886 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+3.0058P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5049 _refine_ls_number_parameters 270 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1430 _refine_ls_wR_factor_gt 0.1421 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6372(3) 0.6111(2) 0.2474(2) 0.0157(4) Uani 1 1 d . . . C2 C 0.4730(3) 0.6578(3) 0.2542(3) 0.0231(5) Uani 1 1 d . B . C3 C 0.4472(4) 0.6834(3) 0.3610(3) 0.0355(8) Uani 1 1 d . . . C4 C 0.5863(5) 0.6587(3) 0.4340(3) 0.0411(9) Uani 1 1 d . B . C5 C 0.7019(4) 0.6169(3) 0.3717(3) 0.0328(7) Uani 1 1 d . B . C6 C 0.6443(3) 0.4744(2) 0.1875(3) 0.0242(5) Uani 1 1 d . B . H6A H 0.5871 0.4731 0.1119 0.036 Uiso 1 1 calc R . . H6B H 0.5970 0.4104 0.2313 0.036 Uiso 1 1 calc R . . H6C H 0.7532 0.4522 0.1809 0.036 Uiso 1 1 calc R . . C7 C 0.3635(4) 0.6701(4) 0.1472(3) 0.0402(8) Uani 1 1 d . . . H7A H 0.3572 0.5866 0.1011 0.060 Uiso 1 1 calc R B . H7B H 0.4030 0.7386 0.1041 0.060 Uiso 1 1 calc R . . H7C H 0.2595 0.6931 0.1673 0.060 Uiso 1 1 calc R . . C8 C 0.2939(5) 0.7292(4) 0.4010(4) 0.0555(12) Uani 1 1 d . B . H8A H 0.2143 0.7297 0.3361 0.083 Uiso 1 1 calc R . . H8B H 0.3080 0.8177 0.4381 0.083 Uiso 1 1 calc R . . H8C H 0.2607 0.6697 0.4548 0.083 Uiso 1 1 calc R . . C9 C 0.5912(7) 0.6776(4) 0.5612(3) 0.0600(13) Uani 1 1 d . . . H9A H 0.5138 0.6194 0.5869 0.090 Uiso 1 1 calc R B . H9B H 0.5677 0.7687 0.5832 0.090 Uiso 1 1 calc R . . H9C H 0.6952 0.6571 0.5959 0.090 Uiso 1 1 calc R . . C10 C 0.8589(5) 0.5765(3) 0.4130(4) 0.0449(9) Uani 1 1 d . . . H10A H 0.9311 0.5942 0.3577 0.067 Uiso 1 1 calc R B . H10B H 0.8574 0.4827 0.4237 0.067 Uiso 1 1 calc R . . H10C H 0.8932 0.6255 0.4852 0.067 Uiso 1 1 calc R . . C11 C 0.7919(3) 0.6750(3) 0.0503(2) 0.0252(6) Uani 1 1 d D . . H11A H 0.7357 0.5914 0.0217 0.030 Uiso 1 1 calc R A 1 C12 C 0.8498(3) 0.7530(3) -0.0394(2) 0.0204(5) Uani 1 1 d . B . H12A H 0.8800 0.8429 -0.0053 0.025 Uiso 1 1 calc R . . C13 C 0.9919(4) 0.6895(4) -0.0821(4) 0.0426(9) Uani 1 1 d . . . H13A H 0.9649 0.6000 -0.1132 0.064 Uiso 1 1 calc R B . H13B H 1.0750 0.6875 -0.0196 0.064 Uiso 1 1 calc R . . H13C H 1.0278 0.7400 -0.1413 0.064 Uiso 1 1 calc R . . C14 C 0.7129(4) 0.7632(4) -0.1298(3) 0.0411(8) Uani 1 1 d . . . H14A H 0.6246 0.8024 -0.0952 0.062 Uiso 1 1 calc R B . H14B H 0.6826 0.6756 -0.1643 0.062 Uiso 1 1 calc R . . H14C H 0.7432 0.8181 -0.1878 0.062 Uiso 1 1 calc R . . C15 C 0.8120(3) 1.1326(3) 0.3110(2) 0.0245(5) Uani 1 1 d . B . C16 C 0.5616(4) 0.9723(3) 0.2945(3) 0.0265(6) Uani 1 1 d . B . C17 C 0.8354(4) 0.9102(3) 0.4060(3) 0.0285(6) Uani 1 1 d . B . C18 C 0.9796(3) 0.9501(3) 0.2183(3) 0.0267(6) Uani 1 1 d . B . C19 C 0.7044(3) 1.0191(3) 0.1128(3) 0.0258(6) Uani 1 1 d . B . O2 O 0.8403(3) 1.2386(2) 0.3437(2) 0.0368(6) Uani 1 1 d . . . O3 O 0.4402(3) 0.9902(2) 0.3199(3) 0.0420(6) Uani 1 1 d . . . O4 O 0.8739(3) 0.8917(2) 0.4978(2) 0.0440(7) Uani 1 1 d . . . O5 O 1.1037(3) 0.9487(2) 0.1939(3) 0.0421(6) Uani 1 1 d . . . O6 O 0.6656(3) 1.0615(2) 0.0284(2) 0.0394(6) Uani 1 1 d . . . O1 O 0.9121(2) 0.6651(2) 0.15452(19) 0.0171(6) Uani 0.800(6) 1 d P B 1 P P 0.7510(2) 0.73945(15) 0.18888(14) 0.0135(3) Uani 0.800(6) 1 d P B 1 O1S O 0.6186(7) 0.7170(11) 0.0308(7) 0.035(3) Uani 0.200(6) 1 d PDU B 2 PS P 0.7036(8) 0.7465(6) 0.1626(5) 0.0133(12) Uani 0.200(6) 1 d PD B 2 Cr Cr 0.77119(5) 0.95833(4) 0.25628(4) 0.01770(13) Uani 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 C1 0.0168(11) 0.0122(10) 0.0182(11) 0.0015(8) 0.0023(9) -0.0019(8) C2 0.0182(12) 0.0171(11) 0.0340(15) -0.0030(10) 0.0069(10) -0.0024(9) C3 0.0502(19) 0.0215(13) 0.0384(17) -0.0041(12) 0.0273(15) -0.0095(13) C4 0.088(3) 0.0176(13) 0.0182(13) -0.0021(10) 0.0154(15) -0.0179(15) C5 0.0443(18) 0.0128(11) 0.0365(16) 0.0094(11) -0.0220(14) -0.0098(11) C6 0.0294(14) 0.0135(11) 0.0313(14) -0.0029(10) 0.0140(11) -0.0029(10) C7 0.0271(15) 0.0345(17) 0.055(2) 0.0017(15) -0.0110(14) 0.0005(13) C8 0.063(3) 0.043(2) 0.068(3) 0.0009(19) 0.045(2) 0.0017(19) C9 0.119(4) 0.038(2) 0.0222(16) 0.0002(14) 0.011(2) -0.020(2) C10 0.046(2) 0.0284(16) 0.056(2) 0.0098(15) -0.0185(17) -0.0004(14) C11 0.0300(14) 0.0187(12) 0.0287(14) -0.0030(10) 0.0153(11) -0.0028(10) C12 0.0216(12) 0.0206(12) 0.0192(12) 0.0010(9) 0.0036(9) -0.0038(9) C13 0.0368(18) 0.0350(17) 0.061(2) 0.0033(16) 0.0301(17) 0.0007(14) C14 0.0441(19) 0.0418(19) 0.0358(17) 0.0094(14) -0.0066(15) -0.0098(15) C15 0.0322(14) 0.0190(12) 0.0244(13) 0.0044(10) 0.0105(11) 0.0015(10) C16 0.0307(14) 0.0158(12) 0.0340(15) 0.0016(10) 0.0081(12) 0.0010(10) C17 0.0328(15) 0.0162(12) 0.0353(16) 0.0024(11) -0.0011(12) -0.0099(11) C18 0.0269(14) 0.0143(11) 0.0398(16) 0.0043(11) 0.0059(12) -0.0004(10) C19 0.0283(14) 0.0173(12) 0.0328(15) 0.0014(11) 0.0076(11) 0.0026(10) O2 0.0639(16) 0.0152(9) 0.0333(12) -0.0018(8) 0.0175(11) -0.0056(10) O3 0.0311(12) 0.0292(12) 0.0693(18) 0.0030(11) 0.0224(12) 0.0073(9) O4 0.0605(16) 0.0328(12) 0.0342(13) 0.0082(10) -0.0173(11) -0.0225(11) O5 0.0244(11) 0.0316(12) 0.0726(18) 0.0049(12) 0.0155(11) -0.0008(9) O6 0.0506(15) 0.0336(12) 0.0348(12) 0.0112(10) 0.0016(11) 0.0068(11) O1 0.0143(10) 0.0173(11) 0.0200(11) 0.0016(8) 0.0033(8) 0.0026(8) P 0.0132(7) 0.0120(4) 0.0154(6) 0.0009(4) 0.0024(5) 0.0006(5) O1S 0.036(3) 0.035(3) 0.034(3) 0.0029(19) 0.0016(19) -0.0016(19) PS 0.013(3) 0.0093(16) 0.019(3) 0.0014(17) 0.0071(19) 0.0014(19) Cr 0.0202(2) 0.0109(2) 0.0230(2) 0.00137(14) 0.00641(16) -0.00010(14) _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. ; 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 C1 C2 1.509(3) . ? C1 C5 1.525(4) . ? C1 C6 1.530(3) . ? C1 P 1.856(3) . ? C1 PS 1.897(7) . ? C2 C3 1.325(4) . ? C2 C7 1.521(4) . ? C3 C4 1.444(6) . ? C3 C8 1.522(5) . ? C4 C5 1.362(5) . ? C4 C9 1.512(4) . ? C5 C10 1.467(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.507(4) . ? C11 O1 1.542(4) . ? C11 O1S 1.560(5) . ? C11 PS 1.732(6) . ? C11 P 1.806(3) . ? C11 H11A 1.0000 . ? C12 C13 1.513(4) . ? C12 C14 1.523(4) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 O2 1.142(4) . ? C15 Cr 1.872(3) . ? C16 O3 1.135(4) . ? C16 Cr 1.917(3) . ? C17 O4 1.141(4) . ? C17 Cr 1.916(3) . ? C18 O5 1.140(4) . ? C18 Cr 1.903(3) . ? C19 O6 1.146(4) . ? C19 Cr 1.901(3) . ? O1 P 1.667(3) . ? P Cr 2.3251(16) . ? O1S PS 1.668(2) . ? PS Cr 2.404(6) . ? 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 C2 C1 C5 102.0(2) . . ? C2 C1 C6 113.3(2) . . ? C5 C1 C6 113.0(2) . . ? C2 C1 P 108.77(18) . . ? C5 C1 P 103.79(18) . . ? C6 C1 P 114.86(18) . . ? C2 C1 PS 96.8(3) . . ? C5 C1 PS 116.4(3) . . ? C6 C1 PS 113.6(2) . . ? P C1 PS 15.19(18) . . ? C3 C2 C1 110.4(3) . . ? C3 C2 C7 129.1(3) . . ? C1 C2 C7 120.5(3) . . ? C2 C3 C4 109.5(3) . . ? C2 C3 C8 125.5(4) . . ? C4 C3 C8 125.0(3) . . ? C5 C4 C3 110.3(3) . . ? C5 C4 C9 128.2(4) . . ? C3 C4 C9 121.5(4) . . ? C4 C5 C10 127.7(3) . . ? C4 C5 C1 107.7(3) . . ? C10 C5 C1 124.5(3) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 O1 113.7(2) . . ? C12 C11 O1S 96.2(4) . . ? O1 C11 O1S 135.3(3) . . ? C12 C11 PS 122.7(3) . . ? O1 C11 PS 75.1(3) . . ? O1S C11 PS 60.64(18) . . ? C12 C11 P 125.9(2) . . ? O1 C11 P 59.10(14) . . ? O1S C11 P 76.6(3) . . ? PS C11 P 16.0(2) . . ? C12 C11 H11A 115.1 . . ? O1 C11 H11A 115.1 . . ? O1S C11 H11A 76.9 . . ? PS C11 H11A 109.4 . . ? P C11 H11A 115.1 . . ? C11 C12 C13 110.0(2) . . ? C11 C12 C14 106.5(2) . . ? C13 C12 C14 114.3(3) . . ? C11 C12 H12A 108.6 . . ? C13 C12 H12A 108.6 . . ? C14 C12 H12A 108.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 Cr 178.4(3) . . ? O3 C16 Cr 174.8(3) . . ? O4 C17 Cr 174.7(3) . . ? O5 C18 Cr 177.8(3) . . ? O6 C19 Cr 176.9(3) . . ? C11 O1 P 68.37(14) . . ? O1 P C11 52.53(13) . . ? O1 P C1 104.71(13) . . ? C11 P C1 106.71(14) . . ? O1 P Cr 118.13(11) . . ? C11 P Cr 125.54(12) . . ? C1 P Cr 125.46(11) . . ? C11 O1S PS 64.8(3) . . ? O1S PS C11 54.6(2) . . ? O1S PS C1 107.0(5) . . ? C11 PS C1 108.1(3) . . ? O1S PS Cr 126.0(5) . . ? C11 PS Cr 125.0(3) . . ? C1 PS Cr 119.4(3) . . ? C15 Cr C19 88.33(12) . . ? C15 Cr C18 88.26(12) . . ? C19 Cr C18 90.25(13) . . ? C15 Cr C17 87.58(12) . . ? C19 Cr C17 175.58(12) . . ? C18 Cr C17 91.30(14) . . ? C15 Cr C16 90.11(12) . . ? C19 Cr C16 89.07(13) . . ? C18 Cr C16 178.26(11) . . ? C17 Cr C16 89.26(14) . . ? C15 Cr P 173.48(10) . . ? C19 Cr P 93.43(10) . . ? C18 Cr P 85.46(9) . . ? C17 Cr P 90.81(9) . . ? C16 Cr P 96.18(9) . . ? C15 Cr PS 172.17(19) . . ? C19 Cr PS 83.89(19) . . ? C18 Cr PS 92.66(18) . . ? C17 Cr PS 100.17(18) . . ? C16 Cr PS 88.87(18) . . ? P Cr PS 11.93(15) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.560 _refine_diff_density_min -0.881 _refine_diff_density_rms 0.094 #------------------------------------------------------------------------------ data_Greg1161 _database_code_depnum_ccdc_archive 'CCDC 792186' #TrackingRef 'Gesamtcif.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H23 Cr O6 P' _chemical_formula_sum 'C19 H23 Cr O6 P' _chemical_formula_weight 430.34 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' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6180(3) _cell_length_b 12.6169(4) _cell_length_c 16.8383(5) _cell_angle_alpha 90.3709(16) _cell_angle_beta 106.2190(15) _cell_angle_gamma 101.5490(18) _cell_volume 2117.46(11) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9638 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 29.13 _exptl_crystal_description parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.6980 _exptl_absorpt_correction_T_max 0.9037 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36206 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.00 _reflns_number_total 10015 _reflns_number_gt 8051 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+1.7837P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10015 _refine_ls_number_parameters 518 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1210 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4394(3) 0.2700(2) 0.71376(15) 0.0328(5) Uani 1 1 d . . . H1 H 0.4403 0.3360 0.7474 0.039 Uiso 1 1 calc R . . C2 C 0.5705(3) 0.2336(2) 0.73398(16) 0.0348(6) Uani 1 1 d . . . H2A H 0.5675 0.1796 0.6902 0.042 Uiso 1 1 calc R . . H2B H 0.5842 0.1981 0.7871 0.042 Uiso 1 1 calc R . . C3 C 0.6861(3) 0.3276(3) 0.7406(2) 0.0478(7) Uani 1 1 d . . . H3A H 0.6866 0.3827 0.7830 0.057 Uiso 1 1 calc R . . H3B H 0.6734 0.3615 0.6869 0.057 Uiso 1 1 calc R . . C4 C 0.8201(4) 0.2940(4) 0.7638(2) 0.0668(10) Uani 1 1 d . . . H4C H 0.8918 0.3574 0.7658 0.100 Uiso 1 1 calc R . . H4B H 0.8201 0.2391 0.7224 0.100 Uiso 1 1 calc R . . H4A H 0.8354 0.2638 0.8183 0.100 Uiso 1 1 calc R . . C5 C 0.2091(2) 0.34796(19) 0.61048(15) 0.0293(5) Uani 1 1 d . . . C6 C 0.0690(2) 0.29242(19) 0.56107(16) 0.0314(5) Uani 1 1 d . . . C7 C 0.0360(2) 0.3395(2) 0.48922(16) 0.0329(5) Uani 1 1 d . . . C8 C 0.1471(3) 0.42726(19) 0.48554(16) 0.0320(5) Uani 1 1 d . . . C9 C 0.2490(2) 0.43306(18) 0.55470(16) 0.0298(5) Uani 1 1 d . . . C10 C 0.2118(3) 0.3926(3) 0.69639(17) 0.0440(7) Uani 1 1 d . . . H10A H 0.1993 0.3323 0.7318 0.066 Uiso 1 1 calc R . . H10B H 0.1395 0.4321 0.6904 0.066 Uiso 1 1 calc R . . H10C H 0.2984 0.4417 0.7217 0.066 Uiso 1 1 calc R . . C11 C -0.0154(3) 0.2029(2) 0.5938(2) 0.0468(7) Uani 1 1 d . . . H11A H -0.0427 0.2327 0.6387 0.070 Uiso 1 1 calc R . . H11B H 0.0368 0.1480 0.6149 0.070 Uiso 1 1 calc R . . H11C H -0.0953 0.1696 0.5490 0.070 Uiso 1 1 calc R . . C12 C -0.0942(3) 0.3137(3) 0.4205(2) 0.0492(7) Uani 1 1 d . . . H12A H -0.1374 0.3761 0.4151 0.074 Uiso 1 1 calc R . . H12B H -0.1537 0.2506 0.4336 0.074 Uiso 1 1 calc R . . H12C H -0.0761 0.2976 0.3683 0.074 Uiso 1 1 calc R . . C13 C 0.1432(3) 0.4985(2) 0.41410(19) 0.0475(7) Uani 1 1 d . . . H13A H 0.0786 0.5448 0.4124 0.071 Uiso 1 1 calc R . . H13B H 0.1159 0.4533 0.3622 0.071 Uiso 1 1 calc R . . H13C H 0.2324 0.5440 0.4212 0.071 Uiso 1 1 calc R . . C14 C 0.3845(3) 0.5081(2) 0.5792(2) 0.0467(7) Uani 1 1 d . . . H14C H 0.3835 0.5692 0.5437 0.070 Uiso 1 1 calc R . . H14B H 0.4523 0.4688 0.5728 0.070 Uiso 1 1 calc R . . H14A H 0.4063 0.5351 0.6372 0.070 Uiso 1 1 calc R . . C15 C 0.3275(3) 0.05708(19) 0.41160(15) 0.0302(5) Uani 1 1 d . . . C16 C 0.5139(3) 0.19320(19) 0.52369(16) 0.0318(5) Uani 1 1 d . . . C17 C 0.3355(3) 0.0316(2) 0.56640(16) 0.0314(5) Uani 1 1 d . . . C18 C 0.1332(3) 0.10757(18) 0.46135(14) 0.0288(5) Uani 1 1 d . . . C19 C 0.3151(2) 0.26584(19) 0.42505(15) 0.0273(5) Uani 1 1 d . . . C21S C 0.0057(6) 0.0865(6) 0.1545(5) 0.0353(16) Uani 0.412(5) 1 d P A 2 H21A H -0.0122 0.1604 0.1477 0.042 Uiso 0.412(5) 1 calc PR A 2 H21B H -0.0410 0.0429 0.1015 0.042 Uiso 0.412(5) 1 calc PR A 2 C20S C 0.1566(3) 0.0924(2) 0.17441(19) 0.0397(6) Uani 0.412(5) 1 d P A 2 H20S H 0.1798 0.0192 0.1794 0.048 Uiso 0.412(5) 1 calc PR A 2 C21 C 0.0464(4) 0.1285(4) 0.2071(3) 0.0314(10) Uani 0.588(5) 1 d P A 1 H21C H 0.0900 0.1746 0.2592 0.038 Uiso 0.588(5) 1 calc PR A 1 H21D H -0.0029 0.1723 0.1659 0.038 Uiso 0.588(5) 1 calc PR A 1 C20 C 0.1566(3) 0.0924(2) 0.17441(19) 0.0397(6) Uani 0.588(5) 1 d P A 1 H20 H 0.2076 0.0445 0.2118 0.048 Uiso 0.588(5) 1 calc PR A 1 C22 C -0.0480(3) 0.0360(3) 0.2225(2) 0.0534(8) Uani 1 1 d . . . H22A H -0.0026 0.0025 0.2725 0.064 Uiso 1 1 calc R A 1 H22B H -0.0742 -0.0185 0.1751 0.064 Uiso 1 1 calc R A 1 C23 C -0.1733(3) 0.0640(3) 0.23484(19) 0.0441(7) Uani 1 1 d . A . H23C H -0.2340 -0.0023 0.2422 0.066 Uiso 1 1 calc R . . H23B H -0.2182 0.0988 0.1862 0.066 Uiso 1 1 calc R . . H23A H -0.1491 0.1138 0.2842 0.066 Uiso 1 1 calc R . . C24 C 0.4103(2) 0.13179(18) 0.12996(14) 0.0254(4) Uani 1 1 d . A . C25 C 0.5242(2) 0.22029(19) 0.17928(15) 0.0278(5) Uani 1 1 d . . . C26 C 0.5949(2) 0.26627(19) 0.12866(17) 0.0313(5) Uani 1 1 d . . . C27 C 0.5334(3) 0.2143(2) 0.04434(16) 0.0322(5) Uani 1 1 d . . . C28 C 0.4270(2) 0.13536(19) 0.04392(15) 0.0293(5) Uani 1 1 d . . . C29 C 0.4126(3) 0.0200(2) 0.16503(18) 0.0359(6) Uani 1 1 d . . . H29A H 0.4051 0.0229 0.2217 0.054 Uiso 1 1 calc R . . H29B H 0.4971 -0.0006 0.1656 0.054 Uiso 1 1 calc R . . H29C H 0.3371 -0.0337 0.1302 0.054 Uiso 1 1 calc R . . C30 C 0.5485(3) 0.2450(2) 0.26989(17) 0.0442(7) Uani 1 1 d . . . H30A H 0.5534 0.1783 0.2990 0.066 Uiso 1 1 calc R . . H30B H 0.4747 0.2751 0.2786 0.066 Uiso 1 1 calc R . . H30C H 0.6332 0.2979 0.2915 0.066 Uiso 1 1 calc R . . C31 C 0.7183(3) 0.3545(2) 0.1513(2) 0.0503(8) Uani 1 1 d . . . H31A H 0.7483 0.3700 0.2116 0.075 Uiso 1 1 calc R . . H31B H 0.6981 0.4200 0.1241 0.075 Uiso 1 1 calc R . . H31C H 0.7892 0.3314 0.1333 0.075 Uiso 1 1 calc R . . C32 C 0.5862(3) 0.2475(3) -0.0277(2) 0.0507(8) Uani 1 1 d . . . H32A H 0.6782 0.2364 -0.0164 0.076 Uiso 1 1 calc R . . H32B H 0.5857 0.3242 -0.0359 0.076 Uiso 1 1 calc R . . H32C H 0.5292 0.2035 -0.0778 0.076 Uiso 1 1 calc R . . C33 C 0.3361(3) 0.0585(2) -0.02611(18) 0.0456(7) Uani 1 1 d . . . H33A H 0.2429 0.0523 -0.0255 0.068 Uiso 1 1 calc R . . H33B H 0.3595 -0.0129 -0.0200 0.068 Uiso 1 1 calc R . . H33C H 0.3463 0.0859 -0.0788 0.068 Uiso 1 1 calc R . . C34 C 0.1584(3) 0.4648(3) 0.0172(3) 0.0577(10) Uani 1 1 d . . . C35 C 0.1411(3) 0.3733(2) 0.15261(19) 0.0386(6) Uani 1 1 d . . . C36 C 0.3766(3) 0.4226(2) 0.1193(2) 0.0448(7) Uani 1 1 d . . . C37 C 0.2613(3) 0.3146(3) -0.0317(2) 0.0498(8) Uani 1 1 d . . . C38 C 0.0309(3) 0.2565(2) 0.00733(18) 0.0419(6) Uani 1 1 d . . . Cr1 Cr 0.32451(4) 0.15004(3) 0.49738(2) 0.02444(10) Uani 1 1 d . . . Cr2 Cr 0.20444(4) 0.33869(3) 0.06302(3) 0.03260(11) Uani 1 1 d . A . O1 O 0.31629(19) 0.18345(14) 0.69991(11) 0.0359(4) Uani 1 1 d . . . O2 O 0.3272(2) -0.00354(15) 0.36030(12) 0.0415(5) Uani 1 1 d . . . O3 O 0.62746(19) 0.21931(17) 0.53506(13) 0.0445(5) Uani 1 1 d . . . O4 O 0.3415(2) -0.04178(16) 0.60577(13) 0.0438(5) Uani 1 1 d . . . O5 O 0.02044(18) 0.07815(14) 0.43466(12) 0.0368(4) Uani 1 1 d . . . O6 O 0.31215(19) 0.33047(14) 0.37764(11) 0.0359(4) Uani 1 1 d . . . O7S O 0.2466(4) 0.1663(3) 0.2251(2) 0.0294(11) Uani 0.412(5) 1 d P A 2 O7 O 0.1291(3) 0.0635(2) 0.09294(19) 0.0320(8) Uani 0.588(5) 1 d P A 1 O8 O 0.1320(3) 0.5431(2) -0.0102(2) 0.0892(10) Uani 1 1 d U . . O9 O 0.1015(2) 0.39799(19) 0.20442(15) 0.0581(6) Uani 1 1 d . . . O10 O 0.4755(2) 0.48013(17) 0.15191(19) 0.0656(7) Uani 1 1 d . . . O11 O 0.2893(3) 0.3066(3) -0.09199(16) 0.0770(9) Uani 1 1 d . . . O12 O -0.0735(2) 0.2075(2) -0.02643(16) 0.0624(6) Uani 1 1 d . . . P1 P 0.31746(6) 0.24889(5) 0.61422(4) 0.02770(14) Uani 1 1 d . . . P2 P 0.25398(6) 0.18023(5) 0.12322(4) 0.02855(14) Uani 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 C1 0.0405(14) 0.0292(12) 0.0293(12) -0.0009(10) 0.0074(10) 0.0124(11) C2 0.0437(14) 0.0349(13) 0.0268(12) 0.0032(10) 0.0053(11) 0.0177(11) C3 0.0432(16) 0.0482(17) 0.0518(18) -0.0005(14) 0.0118(14) 0.0120(13) C4 0.0450(18) 0.090(3) 0.067(2) -0.004(2) 0.0131(17) 0.0224(19) C5 0.0338(12) 0.0272(12) 0.0285(12) -0.0045(9) 0.0069(10) 0.0134(10) C6 0.0293(12) 0.0240(11) 0.0447(14) -0.0058(10) 0.0180(11) 0.0043(9) C7 0.0301(12) 0.0311(12) 0.0376(14) -0.0103(10) 0.0057(10) 0.0129(10) C8 0.0425(14) 0.0263(12) 0.0351(13) 0.0010(10) 0.0164(11) 0.0176(10) C9 0.0298(11) 0.0184(10) 0.0441(14) -0.0033(9) 0.0156(10) 0.0048(9) C10 0.0521(17) 0.0505(17) 0.0345(14) -0.0080(12) 0.0087(12) 0.0283(14) C11 0.0459(16) 0.0403(15) 0.0612(19) 0.0007(14) 0.0311(15) 0.0030(13) C12 0.0392(15) 0.0454(17) 0.0543(18) -0.0128(14) -0.0057(13) 0.0163(13) C13 0.066(2) 0.0408(16) 0.0489(17) 0.0135(13) 0.0255(15) 0.0285(15) C14 0.0369(14) 0.0277(13) 0.073(2) -0.0066(13) 0.0170(14) -0.0008(11) C15 0.0381(13) 0.0248(11) 0.0318(12) 0.0053(10) 0.0129(10) 0.0115(10) C16 0.0388(14) 0.0253(12) 0.0344(13) 0.0029(10) 0.0117(11) 0.0119(10) C17 0.0345(13) 0.0303(12) 0.0324(13) -0.0009(10) 0.0121(10) 0.0105(10) C18 0.0409(14) 0.0221(11) 0.0270(12) 0.0019(9) 0.0132(10) 0.0099(10) C19 0.0262(11) 0.0240(11) 0.0340(12) -0.0027(10) 0.0113(9) 0.0071(9) C21S 0.024(3) 0.039(4) 0.044(4) 0.002(3) 0.015(3) 0.002(3) C20S 0.0306(13) 0.0362(14) 0.0590(18) 0.0198(13) 0.0214(13) 0.0101(11) C21 0.027(2) 0.030(2) 0.038(3) 0.004(2) 0.0120(19) 0.0040(17) C20 0.0306(13) 0.0362(14) 0.0590(18) 0.0198(13) 0.0214(13) 0.0101(11) C22 0.0464(17) 0.072(2) 0.0560(19) 0.0288(17) 0.0294(15) 0.0232(16) C23 0.0319(13) 0.0601(19) 0.0424(16) 0.0003(13) 0.0162(12) 0.0067(13) C24 0.0281(11) 0.0220(11) 0.0285(12) 0.0013(9) 0.0102(9) 0.0078(9) C25 0.0266(11) 0.0260(11) 0.0301(12) -0.0021(9) 0.0030(9) 0.0111(9) C26 0.0245(11) 0.0256(12) 0.0453(14) -0.0012(10) 0.0105(10) 0.0077(9) C27 0.0349(13) 0.0316(13) 0.0383(14) 0.0041(10) 0.0198(11) 0.0128(10) C28 0.0316(12) 0.0283(12) 0.0306(12) -0.0030(9) 0.0108(10) 0.0095(10) C29 0.0368(13) 0.0276(12) 0.0514(16) 0.0103(11) 0.0200(12) 0.0147(10) C30 0.0542(17) 0.0435(16) 0.0312(14) -0.0023(12) 0.0020(12) 0.0169(13) C31 0.0310(14) 0.0354(15) 0.082(2) -0.0045(15) 0.0169(14) -0.0005(12) C32 0.0576(19) 0.0543(18) 0.0566(19) 0.0106(15) 0.0395(16) 0.0162(15) C33 0.0491(16) 0.0459(16) 0.0388(15) -0.0145(13) 0.0107(13) 0.0063(13) C34 0.0318(14) 0.0532(19) 0.103(3) 0.0445(19) 0.0349(17) 0.0204(13) C35 0.0342(13) 0.0281(13) 0.0538(17) 0.0045(12) 0.0110(12) 0.0094(11) C36 0.0354(14) 0.0283(13) 0.076(2) 0.0085(13) 0.0185(14) 0.0141(12) C37 0.0442(16) 0.068(2) 0.0481(18) 0.0293(15) 0.0189(14) 0.0271(15) C38 0.0362(14) 0.0492(17) 0.0404(15) 0.0136(13) 0.0068(12) 0.0150(13) Cr1 0.0299(2) 0.02019(18) 0.02578(19) 0.00033(14) 0.00946(15) 0.00894(14) Cr2 0.0255(2) 0.0316(2) 0.0454(3) 0.01401(18) 0.01331(17) 0.01173(16) O1 0.0446(10) 0.0328(9) 0.0345(10) 0.0048(7) 0.0163(8) 0.0103(8) O2 0.0628(13) 0.0350(10) 0.0348(10) 0.0006(8) 0.0195(9) 0.0210(9) O3 0.0338(10) 0.0461(11) 0.0547(12) 0.0067(9) 0.0139(9) 0.0091(9) O4 0.0565(12) 0.0350(10) 0.0462(11) 0.0150(9) 0.0193(10) 0.0171(9) O5 0.0353(10) 0.0303(9) 0.0412(10) -0.0015(8) 0.0081(8) 0.0028(8) O6 0.0426(10) 0.0310(9) 0.0406(10) 0.0077(8) 0.0189(8) 0.0128(8) O7S 0.029(2) 0.036(2) 0.027(2) 0.0032(17) 0.0132(17) 0.0097(18) O7 0.0277(15) 0.0287(16) 0.0369(17) 0.0003(12) 0.0078(12) 0.0013(12) O8 0.0519(14) 0.0736(17) 0.167(3) 0.0781(18) 0.0556(16) 0.0328(13) O9 0.0622(14) 0.0564(14) 0.0642(15) -0.0066(11) 0.0245(12) 0.0231(12) O10 0.0369(12) 0.0317(11) 0.122(2) -0.0105(12) 0.0149(13) 0.0043(9) O11 0.0810(18) 0.125(2) 0.0509(14) 0.0421(15) 0.0346(14) 0.0566(18) O12 0.0405(12) 0.0670(16) 0.0630(15) 0.0063(12) -0.0082(11) 0.0058(11) P1 0.0321(3) 0.0243(3) 0.0282(3) -0.0004(2) 0.0090(2) 0.0091(2) P2 0.0270(3) 0.0269(3) 0.0376(3) 0.0085(3) 0.0153(3) 0.0102(2) _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. ; 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 C1 O1 1.487(3) . ? C1 C2 1.503(4) . ? C1 P1 1.789(3) . ? C1 H1 1.0000 . ? C2 C3 1.506(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.513(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4C 0.9800 . ? C4 H4B 0.9800 . ? C4 H4A 0.9800 . ? C5 C9 1.506(3) . ? C5 C6 1.510(3) . ? C5 C10 1.540(3) . ? C5 P1 1.851(2) . ? C6 C7 1.340(4) . ? C6 C11 1.503(4) . ? C7 C8 1.463(4) . ? C7 C12 1.509(4) . ? C8 C9 1.340(4) . ? C8 C13 1.503(4) . ? C9 C14 1.501(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14C 0.9800 . ? C14 H14B 0.9800 . ? C14 H14A 0.9800 . ? C15 O2 1.149(3) . ? C15 Cr1 1.866(2) . ? C16 O3 1.145(3) . ? C16 Cr1 1.897(3) . ? C17 O4 1.144(3) . ? C17 Cr1 1.901(3) . ? C18 O5 1.137(3) . ? C18 Cr1 1.911(3) . ? C19 O6 1.144(3) . ? C19 Cr1 1.908(2) . ? C21S C22 1.507(7) . ? C21S C20S 1.528(6) . ? C21S H21A 0.9900 . ? C21S H21B 0.9900 . ? C20S O7S 1.300(5) . ? C20S P2 1.759(3) . ? C20S H20S 1.0000 . ? C21 C22 1.454(5) . ? C21 H21C 0.9900 . ? C21 H21D 0.9900 . ? C22 C23 1.510(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23C 0.9800 . ? C23 H23B 0.9800 . ? C23 H23A 0.9800 . ? C24 C28 1.508(3) . ? C24 C25 1.512(3) . ? C24 C29 1.535(3) . ? C24 P2 1.856(2) . ? C25 C26 1.348(3) . ? C25 C30 1.495(4) . ? C26 C27 1.473(4) . ? C26 C31 1.494(4) . ? C27 C28 1.347(3) . ? C27 C32 1.501(4) . ? C28 C33 1.496(4) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 O8 1.145(4) . ? C34 Cr2 1.866(3) . ? C35 O9 1.136(4) . ? C35 Cr2 1.896(3) . ? C36 O10 1.140(4) . ? C36 Cr2 1.899(3) . ? C37 O11 1.143(4) . ? C37 Cr2 1.899(3) . ? C38 O12 1.141(4) . ? C38 Cr2 1.899(3) . ? Cr1 P1 2.3494(7) . ? Cr2 P2 2.3346(7) . ? O1 P1 1.6688(18) . ? O7S P2 1.747(4) . ? O7 P2 1.738(3) . ? 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 O1 C1 C2 116.4(2) . . ? O1 C1 P1 60.42(12) . . ? C2 C1 P1 124.54(18) . . ? O1 C1 H1 114.7 . . ? C2 C1 H1 114.7 . . ? P1 C1 H1 114.7 . . ? C1 C2 C3 111.3(2) . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C2 C3 C4 112.5(3) . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C3 C4 H4C 109.5 . . ? C3 C4 H4B 109.5 . . ? H4C C4 H4B 109.5 . . ? C3 C4 H4A 109.5 . . ? H4C C4 H4A 109.5 . . ? H4B C4 H4A 109.5 . . ? C9 C5 C6 103.0(2) . . ? C9 C5 C10 114.6(2) . . ? C6 C5 C10 111.5(2) . . ? C9 C5 P1 106.01(16) . . ? C6 C5 P1 106.89(15) . . ? C10 C5 P1 113.93(17) . . ? C7 C6 C11 128.6(3) . . ? C7 C6 C5 108.8(2) . . ? C11 C6 C5 122.5(2) . . ? C6 C7 C8 109.6(2) . . ? C6 C7 C12 128.3(3) . . ? C8 C7 C12 122.1(3) . . ? C9 C8 C7 109.5(2) . . ? C9 C8 C13 126.7(3) . . ? C7 C8 C13 123.8(3) . . ? C8 C9 C14 129.5(3) . . ? C8 C9 C5 109.0(2) . . ? C14 C9 C5 121.4(2) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14C 109.5 . . ? C9 C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? C9 C14 H14A 109.5 . . ? H14C C14 H14A 109.5 . . ? H14B C14 H14A 109.5 . . ? O2 C15 Cr1 177.3(2) . . ? O3 C16 Cr1 176.3(2) . . ? O4 C17 Cr1 177.9(2) . . ? O5 C18 Cr1 174.6(2) . . ? O6 C19 Cr1 174.8(2) . . ? C22 C21S C20S 110.9(5) . . ? C22 C21S H21A 109.5 . . ? C20S C21S H21A 109.5 . . ? C22 C21S H21B 109.5 . . ? C20S C21S H21B 109.5 . . ? H21A C21S H21B 108.0 . . ? O7S C20S C21S 123.6(4) . . ? O7S C20S P2 67.8(2) . . ? C21S C20S P2 120.5(3) . . ? O7S C20S H20S 112.6 . . ? C21S C20S H20S 112.6 . . ? P2 C20S H20S 112.6 . . ? C22 C21 H21C 109.3 . . ? C22 C21 H21D 109.3 . . ? H21C C21 H21D 107.9 . . ? C21 C22 C21S 38.2(3) . . ? C21 C22 C23 113.9(3) . . ? C21S C22 C23 118.9(3) . . ? C21 C22 H22A 108.8 . . ? C21S C22 H22A 129.9 . . ? C23 C22 H22A 108.8 . . ? C21 C22 H22B 108.8 . . ? C21S C22 H22B 71.7 . . ? C23 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C22 C23 H23C 109.5 . . ? C22 C23 H23B 109.5 . . ? H23C C23 H23B 109.5 . . ? C22 C23 H23A 109.5 . . ? H23C C23 H23A 109.5 . . ? H23B C23 H23A 109.5 . . ? C28 C24 C25 103.44(19) . . ? C28 C24 C29 112.82(19) . . ? C25 C24 C29 113.4(2) . . ? C28 C24 P2 105.98(16) . . ? C25 C24 P2 106.04(15) . . ? C29 C24 P2 114.27(16) . . ? C26 C25 C30 128.9(2) . . ? C26 C25 C24 108.8(2) . . ? C30 C25 C24 122.3(2) . . ? C25 C26 C27 109.4(2) . . ? C25 C26 C31 127.3(3) . . ? C27 C26 C31 123.3(2) . . ? C28 C27 C26 109.5(2) . . ? C28 C27 C32 127.3(3) . . ? C26 C27 C32 123.2(2) . . ? C27 C28 C33 129.1(2) . . ? C27 C28 C24 108.9(2) . . ? C33 C28 C24 122.0(2) . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O8 C34 Cr2 178.9(4) . . ? O9 C35 Cr2 176.8(2) . . ? O10 C36 Cr2 174.5(2) . . ? O11 C37 Cr2 174.0(3) . . ? O12 C38 Cr2 179.6(3) . . ? C15 Cr1 C16 88.88(11) . . ? C15 Cr1 C17 87.63(10) . . ? C16 Cr1 C17 92.25(11) . . ? C15 Cr1 C19 90.25(10) . . ? C16 Cr1 C19 87.25(10) . . ? C17 Cr1 C19 177.83(10) . . ? C15 Cr1 C18 87.69(10) . . ? C16 Cr1 C18 175.21(10) . . ? C17 Cr1 C18 90.95(10) . . ? C19 Cr1 C18 89.42(10) . . ? C15 Cr1 P1 173.26(7) . . ? C16 Cr1 P1 92.57(8) . . ? C17 Cr1 P1 85.74(7) . . ? C19 Cr1 P1 96.39(7) . . ? C18 Cr1 P1 91.22(7) . . ? C34 Cr2 C35 87.34(14) . . ? C34 Cr2 C36 88.40(14) . . ? C35 Cr2 C36 89.35(13) . . ? C34 Cr2 C37 87.47(15) . . ? C35 Cr2 C37 174.75(12) . . ? C36 Cr2 C37 91.26(15) . . ? C34 Cr2 C38 90.99(14) . . ? C35 Cr2 C38 89.89(12) . . ? C36 Cr2 C38 179.04(13) . . ? C37 Cr2 C38 89.44(14) . . ? C34 Cr2 P2 177.32(9) . . ? C35 Cr2 P2 90.34(8) . . ? C36 Cr2 P2 92.91(8) . . ? C37 Cr2 P2 94.83(9) . . ? C38 Cr2 P2 87.67(9) . . ? C1 O1 P1 68.79(12) . . ? C20S O7S P2 68.7(2) . . ? O1 P1 C1 50.79(11) . . ? O1 P1 C5 105.86(10) . . ? C1 P1 C5 107.14(11) . . ? O1 P1 Cr1 117.93(7) . . ? C1 P1 Cr1 126.86(8) . . ? C5 P1 Cr1 124.17(8) . . ? O7 P2 O7S 88.90(17) . . ? O7 P2 C20S 45.48(14) . . ? O7S P2 C20S 43.52(17) . . ? O7 P2 C24 103.51(12) . . ? O7S P2 C24 100.03(15) . . ? C20S P2 C24 108.98(11) . . ? O7 P2 Cr2 116.48(10) . . ? O7S P2 Cr2 116.65(14) . . ? C20S P2 Cr2 126.35(9) . . ? C24 P2 Cr2 124.56(8) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.506 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.124 #------------------------------------------------------------------------------ data_Greg742 _database_code_depnum_ccdc_archive 'CCDC 792187' #TrackingRef 'Gesamtcif.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H21 Cr O6 P' _chemical_formula_sum 'C22 H21 Cr O6 P' _chemical_formula_weight 464.36 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' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5334(3) _cell_length_b 10.1367(4) _cell_length_c 13.1037(5) _cell_angle_alpha 101.172(2) _cell_angle_beta 110.283(2) _cell_angle_gamma 102.683(2) _cell_volume 1107.27(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4032 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 29.13 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 1.19 _exptl_crystal_size_mid 0.91 _exptl_crystal_size_min 0.84 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 0.623 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.50381 _exptl_absorpt_correction_T_max 0.76911 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14121 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5159 _reflns_number_gt 4444 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.3119P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5159 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.25506(18) 0.60779(17) 0.62134(13) 0.0237(3) Uani 1 1 d . . . H1A H 0.2038 0.5242 0.6402 0.028 Uiso 1 1 calc R . . C2 C 0.14738(18) 0.68229(16) 0.56396(13) 0.0239(3) Uani 1 1 d . . . C3 C 0.0284(2) 0.6975(2) 0.59860(16) 0.0340(4) Uani 1 1 d . . . H3A H 0.0175 0.6614 0.6581 0.041 Uiso 1 1 calc R . . C4 C -0.0745(2) 0.7653(2) 0.54642(18) 0.0397(4) Uani 1 1 d . . . H4A H -0.1559 0.7754 0.5703 0.048 Uiso 1 1 calc R . . C5 C -0.0600(2) 0.81809(19) 0.46041(17) 0.0381(4) Uani 1 1 d . . . H5A H -0.1304 0.8655 0.4256 0.046 Uiso 1 1 calc R . . C6 C 0.0570(2) 0.80218(19) 0.42462(15) 0.0344(4) Uani 1 1 d . . . H6A H 0.0665 0.8379 0.3646 0.041 Uiso 1 1 calc R . . C7 C 0.16123(19) 0.73386(18) 0.47628(14) 0.0280(3) Uani 1 1 d . . . H7A H 0.2416 0.7227 0.4514 0.034 Uiso 1 1 calc R . . C8 C 0.53006(18) 0.57655(16) 0.79678(12) 0.0210(3) Uani 1 1 d . . . C9 C 0.56762(19) 0.65145(16) 0.91941(13) 0.0230(3) Uani 1 1 d . . . C10 C 0.7245(2) 0.68876(16) 0.97957(13) 0.0255(3) Uani 1 1 d . . . C11 C 0.79969(18) 0.64300(17) 0.90323(14) 0.0254(3) Uani 1 1 d . . . C12 C 0.68916(19) 0.57979(16) 0.79691(13) 0.0231(3) Uani 1 1 d . . . C13 C 0.4165(2) 0.42550(17) 0.75291(15) 0.0298(4) Uani 1 1 d . . . H13A H 0.3226 0.4262 0.7677 0.045 Uiso 1 1 calc R . . H13B H 0.4684 0.3653 0.7921 0.045 Uiso 1 1 calc R . . H13C H 0.3857 0.3884 0.6708 0.045 Uiso 1 1 calc R . . C14 C 0.4429(2) 0.6721(2) 0.95913(16) 0.0338(4) Uani 1 1 d . . . H14A H 0.3827 0.5812 0.9605 0.051 Uiso 1 1 calc R . . H14B H 0.3721 0.7098 0.9071 0.051 Uiso 1 1 calc R . . H14C H 0.4918 0.7390 1.0359 0.051 Uiso 1 1 calc R . . C15 C 0.8169(2) 0.7629(2) 1.10385(15) 0.0377(4) Uani 1 1 d . . . H15A H 0.8715 0.7021 1.1401 0.057 Uiso 1 1 calc R . . H15B H 0.7455 0.7840 1.1388 0.057 Uiso 1 1 calc R . . H15C H 0.8943 0.8514 1.1141 0.057 Uiso 1 1 calc R . . C16 C 0.9737(2) 0.6675(2) 0.94461(17) 0.0403(4) Uani 1 1 d . . . H16A H 1.0072 0.6222 1.0046 0.060 Uiso 1 1 calc R . . H16B H 1.0293 0.7694 0.9751 0.060 Uiso 1 1 calc R . . H16C H 0.9983 0.6269 0.8812 0.060 Uiso 1 1 calc R . . C17 C 0.7080(2) 0.51608(19) 0.69127(15) 0.0313(4) Uani 1 1 d . . . H17A H 0.6902 0.5759 0.6406 0.047 Uiso 1 1 calc R . . H17B H 0.6314 0.4213 0.6523 0.047 Uiso 1 1 calc R . . H17C H 0.8147 0.5094 0.7118 0.047 Uiso 1 1 calc R . . C18 C 0.64181(19) 0.97602(17) 0.90825(15) 0.0272(3) Uani 1 1 d . . . C19 C 0.7986(2) 0.89882(17) 0.78569(15) 0.0285(4) Uani 1 1 d . . . C20 C 0.56870(19) 0.88709(17) 0.59365(15) 0.0269(3) Uani 1 1 d . . . C21 C 0.4122(2) 0.98268(17) 0.72145(14) 0.0283(3) Uani 1 1 d . . . C22 C 0.6994(2) 1.12018(18) 0.76756(14) 0.0297(4) Uani 1 1 d . . . Cr Cr 0.60010(3) 0.93087(2) 0.74960(2) 0.02153(9) Uani 1 1 d . . . O1 O 0.37409(13) 0.58912(12) 0.57754(9) 0.0240(2) Uani 1 1 d . . . O2 O 0.67129(16) 1.01079(13) 1.00320(11) 0.0366(3) Uani 1 1 d . . . O3 O 0.92259(15) 0.89054(14) 0.80758(13) 0.0421(3) Uani 1 1 d . . . O4 O 0.55617(16) 0.86296(14) 0.50160(11) 0.0371(3) Uani 1 1 d . . . O5 O 0.30872(16) 1.02604(14) 0.71068(12) 0.0410(3) Uani 1 1 d . . . O6 O 0.75763(17) 1.23490(14) 0.77559(12) 0.0437(3) Uani 1 1 d . . . P P 0.46119(4) 0.69416(4) 0.71135(3) 0.01947(10) Uani 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 C1 0.0228(7) 0.0208(8) 0.0225(8) 0.0047(6) 0.0059(6) 0.0043(6) C2 0.0205(7) 0.0167(8) 0.0226(8) -0.0008(6) 0.0011(6) 0.0017(6) C3 0.0251(8) 0.0335(10) 0.0373(10) 0.0071(8) 0.0095(7) 0.0059(7) C4 0.0242(9) 0.0346(10) 0.0498(12) 0.0020(9) 0.0087(8) 0.0091(7) C5 0.0251(9) 0.0215(9) 0.0458(11) 0.0001(8) -0.0058(8) 0.0074(7) C6 0.0355(9) 0.0269(9) 0.0281(9) 0.0067(7) 0.0000(7) 0.0081(7) C7 0.0270(8) 0.0263(9) 0.0225(8) 0.0034(6) 0.0031(7) 0.0076(7) C8 0.0255(7) 0.0139(7) 0.0175(7) 0.0052(6) 0.0036(6) 0.0026(6) C9 0.0315(8) 0.0149(7) 0.0210(7) 0.0065(6) 0.0097(6) 0.0046(6) C10 0.0340(9) 0.0162(8) 0.0189(7) 0.0065(6) 0.0055(7) 0.0014(6) C11 0.0259(8) 0.0208(8) 0.0267(8) 0.0111(6) 0.0063(7) 0.0056(6) C12 0.0296(8) 0.0162(7) 0.0232(8) 0.0081(6) 0.0092(6) 0.0074(6) C13 0.0319(9) 0.0168(8) 0.0287(9) 0.0078(7) 0.0034(7) -0.0012(6) C14 0.0418(10) 0.0334(10) 0.0329(9) 0.0142(8) 0.0206(8) 0.0119(8) C15 0.0462(11) 0.0298(10) 0.0210(8) 0.0045(7) 0.0050(8) -0.0021(8) C16 0.0282(9) 0.0453(12) 0.0417(11) 0.0210(9) 0.0051(8) 0.0086(8) C17 0.0414(10) 0.0266(9) 0.0283(9) 0.0074(7) 0.0149(8) 0.0148(8) C18 0.0289(8) 0.0168(8) 0.0304(9) 0.0073(6) 0.0066(7) 0.0055(6) C19 0.0302(9) 0.0168(8) 0.0313(9) 0.0096(7) 0.0066(7) 0.0015(6) C20 0.0272(8) 0.0193(8) 0.0314(9) 0.0101(7) 0.0083(7) 0.0055(6) C21 0.0325(9) 0.0200(8) 0.0224(8) 0.0027(6) 0.0034(7) 0.0050(7) C22 0.0323(9) 0.0240(9) 0.0253(8) 0.0097(7) 0.0031(7) 0.0063(7) Cr 0.02355(14) 0.01453(14) 0.02111(14) 0.00641(10) 0.00371(11) 0.00353(10) O1 0.0266(6) 0.0223(6) 0.0185(5) 0.0029(4) 0.0051(4) 0.0084(5) O2 0.0485(8) 0.0276(7) 0.0259(7) 0.0042(5) 0.0097(6) 0.0096(6) O3 0.0254(7) 0.0350(8) 0.0645(10) 0.0239(7) 0.0131(6) 0.0075(5) O4 0.0455(8) 0.0384(8) 0.0301(7) 0.0132(6) 0.0164(6) 0.0138(6) O5 0.0373(7) 0.0341(8) 0.0411(8) 0.0020(6) 0.0045(6) 0.0184(6) O6 0.0461(8) 0.0225(7) 0.0451(8) 0.0150(6) 0.0024(6) -0.0003(6) P 0.0212(2) 0.0155(2) 0.01732(19) 0.00466(15) 0.00413(15) 0.00353(15) _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. ; 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 C1 O1 1.4685(19) . ? C1 C2 1.488(2) . ? C1 P 1.8046(16) . ? C1 H1A 1.0000 . ? C2 C7 1.385(2) . ? C2 C3 1.387(2) . ? C3 C4 1.384(3) . ? C3 H3A 0.9500 . ? C4 C5 1.373(3) . ? C4 H4A 0.9500 . ? C5 C6 1.379(3) . ? C5 H5A 0.9500 . ? C6 C7 1.394(2) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C12 1.509(2) . ? C8 C9 1.515(2) . ? C8 C13 1.532(2) . ? C8 P 1.8592(15) . ? C9 C10 1.349(2) . ? C9 C14 1.492(2) . ? C10 C11 1.481(2) . ? C10 C15 1.494(2) . ? C11 C12 1.342(2) . ? C11 C16 1.500(2) . ? C12 C17 1.497(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O2 1.138(2) . ? C18 Cr 1.9152(18) . ? C19 O3 1.142(2) . ? C19 Cr 1.9021(18) . ? C20 O4 1.141(2) . ? C20 Cr 1.9048(18) . ? C21 O5 1.142(2) . ? C21 Cr 1.9106(18) . ? C22 O6 1.140(2) . ? C22 Cr 1.8726(17) . ? Cr P 2.3326(5) . ? O1 P 1.6662(11) . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.598 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.055 #------------------------------------------------------------------------------ data_Greg1001 _database_code_depnum_ccdc_archive 'CCDC 792188' #TrackingRef 'Gesamtcif.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H25 Cr O6 P' _chemical_formula_sum 'C20 H25 Cr O6 P' _chemical_formula_weight 444.37 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' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7299(4) _cell_length_b 10.5893(5) _cell_length_c 11.8257(6) _cell_angle_alpha 85.069(3) _cell_angle_beta 83.532(3) _cell_angle_gamma 89.728(3) _cell_volume 1082.22(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4170 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 30.03 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 0.634 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.71917 _exptl_absorpt_correction_T_max 0.94781 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13428 _diffrn_reflns_av_R_equivalents 0.0919 _diffrn_reflns_av_sigmaI/netI 0.0917 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5173 _reflns_number_gt 3634 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5173 _refine_ls_number_parameters 261 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8597(3) 0.8790(2) 0.2460(2) 0.0243(5) Uani 1 1 d . . . C2 C 1.0234(3) 0.8338(2) 0.2478(2) 0.0255(5) Uani 1 1 d . . . C3 C 1.0555(3) 0.8142(2) 0.3558(2) 0.0290(6) Uani 1 1 d . . . C4 C 0.9158(3) 0.8407(2) 0.4334(2) 0.0294(6) Uani 1 1 d . . . C5 C 0.8010(3) 0.8763(2) 0.3722(2) 0.0267(5) Uani 1 1 d . . . C6 C 0.8511(3) 1.0147(2) 0.1885(2) 0.0344(6) Uani 1 1 d . . . H6A H 0.9136 1.0205 0.1140 0.052 Uiso 1 1 calc R . . H6B H 0.8905 1.0747 0.2370 0.052 Uiso 1 1 calc R . . H6C H 0.7437 1.0350 0.1780 0.052 Uiso 1 1 calc R . . C7 C 1.1279(3) 0.8153(3) 0.1401(2) 0.0409(7) Uani 1 1 d . . . H7A H 1.1212 0.8892 0.0850 0.061 Uiso 1 1 calc R . . H7B H 1.0961 0.7392 0.1071 0.061 Uiso 1 1 calc R . . H7C H 1.2345 0.8055 0.1580 0.061 Uiso 1 1 calc R . . C8 C 1.2058(3) 0.7762(3) 0.3978(3) 0.0483(8) Uani 1 1 d . . . H8A H 1.2861 0.7763 0.3328 0.072 Uiso 1 1 calc R . . H8B H 1.1960 0.6910 0.4375 0.072 Uiso 1 1 calc R . . H8C H 1.2337 0.8364 0.4506 0.072 Uiso 1 1 calc R . . C9 C 0.9125(4) 0.8286(3) 0.5609(2) 0.0472(8) Uani 1 1 d . . . H9A H 0.9833 0.8908 0.5837 0.071 Uiso 1 1 calc R . . H9B H 0.9443 0.7429 0.5865 0.071 Uiso 1 1 calc R . . H9C H 0.8077 0.8441 0.5959 0.071 Uiso 1 1 calc R . . C10 C 0.6419(3) 0.9191(3) 0.4121(3) 0.0431(7) Uani 1 1 d . . . H10A H 0.5669 0.8771 0.3720 0.065 Uiso 1 1 calc R . . H10B H 0.6349 1.0112 0.3958 0.065 Uiso 1 1 calc R . . H10C H 0.6198 0.8972 0.4945 0.065 Uiso 1 1 calc R . . C11 C 0.7120(3) 0.8290(2) 0.0461(2) 0.0297(6) Uani 1 1 d . . . H11A H 0.7697 0.9106 0.0259 0.036 Uiso 1 1 calc R . . C12 C 0.6620(3) 0.7747(2) -0.0594(2) 0.0321(6) Uani 1 1 d . . . C13 C 0.5426(3) 0.6693(2) -0.0314(2) 0.0325(6) Uani 1 1 d . . . H13A H 0.4531 0.7002 0.0159 0.049 Uiso 1 1 calc R . . H13B H 0.5877 0.5970 0.0104 0.049 Uiso 1 1 calc R . . H13C H 0.5100 0.6426 -0.1024 0.049 Uiso 1 1 calc R . . C14 C 0.5924(5) 0.8839(3) -0.1297(3) 0.0677(11) Uani 1 1 d . . . H14A H 0.6707 0.9499 -0.1529 0.101 Uiso 1 1 calc R . . H14B H 0.5050 0.9194 -0.0835 0.101 Uiso 1 1 calc R . . H14C H 0.5569 0.8524 -0.1979 0.101 Uiso 1 1 calc R . . C15 C 0.8056(3) 0.7256(3) -0.1278(2) 0.0459(8) Uani 1 1 d . . . H15C H 0.7773 0.6946 -0.1984 0.069 Uiso 1 1 calc R . . H15B H 0.8505 0.6563 -0.0822 0.069 Uiso 1 1 calc R . . H15A H 0.8812 0.7945 -0.1467 0.069 Uiso 1 1 calc R . . C16 C 0.6889(3) 0.3780(2) 0.3186(2) 0.0306(6) Uani 1 1 d . . . C17 C 0.5138(3) 0.5556(2) 0.2408(2) 0.0277(6) Uani 1 1 d . . . C18 C 0.7945(3) 0.4838(2) 0.1238(2) 0.0273(5) Uani 1 1 d . . . C19 C 0.9311(3) 0.5330(2) 0.3044(2) 0.0307(6) Uani 1 1 d . . . C20 C 0.6666(3) 0.5943(2) 0.4169(2) 0.0318(6) Uani 1 1 d . . . Cr Cr 0.72502(4) 0.54747(3) 0.26566(3) 0.02198(13) Uani 1 1 d . . . O1 O 0.59387(19) 0.83759(16) 0.14551(15) 0.0325(4) Uani 1 1 d . . . O2 O 0.6643(2) 0.27271(17) 0.34542(17) 0.0451(5) Uani 1 1 d . . . O3 O 0.3855(2) 0.55650(19) 0.23066(17) 0.0422(5) Uani 1 1 d . . . O4 O 0.8390(2) 0.43621(19) 0.04334(16) 0.0417(5) Uani 1 1 d . . . O5 O 1.0501(2) 0.51326(19) 0.33257(19) 0.0473(5) Uani 1 1 d . . . O6 O 0.6316(2) 0.61248(19) 0.51008(16) 0.0473(5) Uani 1 1 d . . . P P 0.74813(7) 0.75791(5) 0.18375(5) 0.02260(16) Uani 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 C1 0.0326(13) 0.0167(11) 0.0241(12) -0.0023(9) -0.0055(10) -0.0080(9) C2 0.0285(12) 0.0215(12) 0.0267(13) -0.0077(10) 0.0004(10) -0.0081(10) C3 0.0356(14) 0.0227(13) 0.0304(14) -0.0061(10) -0.0083(11) -0.0019(10) C4 0.0496(15) 0.0190(12) 0.0198(12) -0.0030(9) -0.0032(11) -0.0067(11) C5 0.0335(13) 0.0179(12) 0.0278(13) -0.0068(10) 0.0046(10) -0.0069(10) C6 0.0518(16) 0.0191(12) 0.0344(15) 0.0014(11) -0.0169(12) -0.0111(11) C7 0.0371(15) 0.0486(17) 0.0358(16) -0.0135(13) 0.0089(12) -0.0143(13) C8 0.0515(18) 0.0456(18) 0.055(2) -0.0186(15) -0.0274(14) 0.0086(14) C9 0.086(2) 0.0335(16) 0.0227(14) -0.0052(12) -0.0057(14) -0.0078(15) C10 0.0381(15) 0.0332(16) 0.0571(19) -0.0155(13) 0.0078(13) -0.0008(12) C11 0.0392(14) 0.0195(12) 0.0318(14) 0.0009(10) -0.0124(11) -0.0071(10) C12 0.0453(15) 0.0213(13) 0.0320(14) -0.0010(10) -0.0148(11) -0.0075(11) C13 0.0327(13) 0.0312(14) 0.0363(15) -0.0135(11) -0.0078(11) -0.0043(11) C14 0.119(3) 0.0293(17) 0.067(2) -0.0024(15) -0.066(2) -0.0031(18) C15 0.0477(17) 0.060(2) 0.0292(15) -0.0004(14) -0.0005(12) -0.0250(15) C16 0.0396(14) 0.0251(13) 0.0275(13) -0.0047(10) -0.0037(11) -0.0028(11) C17 0.0333(14) 0.0161(12) 0.0325(14) -0.0100(10) 0.0082(11) -0.0023(10) C18 0.0268(12) 0.0227(13) 0.0317(14) -0.0021(11) -0.0005(10) 0.0014(10) C19 0.0377(15) 0.0174(12) 0.0362(15) -0.0026(10) -0.0010(12) -0.0015(11) C20 0.0348(14) 0.0233(13) 0.0357(15) -0.0023(11) 0.0034(12) -0.0107(11) Cr 0.0254(2) 0.0146(2) 0.0252(2) -0.00368(15) 0.00216(15) -0.00251(14) O1 0.0359(9) 0.0223(9) 0.0424(11) -0.0093(8) -0.0133(8) 0.0044(7) O2 0.0717(14) 0.0211(10) 0.0430(12) 0.0025(8) -0.0120(10) -0.0074(9) O3 0.0267(10) 0.0452(12) 0.0544(13) -0.0150(10) 0.0049(9) -0.0035(8) O4 0.0421(11) 0.0481(12) 0.0356(11) -0.0158(9) 0.0019(9) 0.0100(9) O5 0.0352(11) 0.0347(11) 0.0736(16) -0.0022(10) -0.0149(10) 0.0048(9) O6 0.0654(13) 0.0429(12) 0.0307(11) -0.0114(9) 0.0149(10) -0.0204(10) P 0.0265(3) 0.0159(3) 0.0260(3) -0.0022(2) -0.0047(2) -0.0036(2) _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. ; 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 C1 C2 1.507(3) . ? C1 C5 1.521(3) . ? C1 C6 1.541(3) . ? C1 P 1.863(2) . ? C2 C3 1.336(3) . ? C2 C7 1.508(3) . ? C3 C4 1.482(4) . ? C3 C8 1.496(4) . ? C4 C5 1.335(4) . ? C4 C9 1.500(3) . ? C5 C10 1.497(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 O1 1.482(3) . ? C11 C12 1.525(4) . ? C11 P 1.794(2) . ? C11 H11A 1.0000 . ? C12 C13 1.520(3) . ? C12 C15 1.528(4) . ? C12 C14 1.530(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15C 0.9800 . ? C15 H15B 0.9800 . ? C15 H15A 0.9800 . ? C16 O2 1.147(3) . ? C16 Cr 1.865(2) . ? C17 O3 1.140(3) . ? C17 Cr 1.900(3) . ? C18 O4 1.143(3) . ? C18 Cr 1.897(3) . ? C19 O5 1.139(3) . ? C19 Cr 1.908(3) . ? C20 O6 1.142(3) . ? C20 Cr 1.911(3) . ? Cr P 2.3524(6) . ? O1 P 1.6706(18) . ? 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 C2 C1 C5 102.79(19) . . ? C2 C1 C6 112.24(18) . . ? C5 C1 C6 110.2(2) . . ? C2 C1 P 108.59(16) . . ? C5 C1 P 107.32(13) . . ? C6 C1 P 114.93(17) . . ? C3 C2 C1 109.7(2) . . ? C3 C2 C7 128.0(2) . . ? C1 C2 C7 122.3(2) . . ? C2 C3 C4 108.9(2) . . ? C2 C3 C8 128.1(2) . . ? C4 C3 C8 122.9(2) . . ? C5 C4 C3 109.7(2) . . ? C5 C4 C9 127.6(2) . . ? C3 C4 C9 122.7(2) . . ? C4 C5 C10 129.3(2) . . ? C4 C5 C1 108.8(2) . . ? C10 C5 C1 121.7(2) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 C12 117.6(2) . . ? O1 C11 P 60.43(11) . . ? C12 C11 P 132.80(17) . . ? O1 C11 H11A 111.6 . . ? C12 C11 H11A 111.6 . . ? P C11 H11A 111.6 . . ? C13 C12 C11 113.4(2) . . ? C13 C12 C15 110.0(2) . . ? C11 C12 C15 107.9(2) . . ? C13 C12 C14 108.8(2) . . ? C11 C12 C14 107.0(2) . . ? C15 C12 C14 109.7(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15C 109.5 . . ? C12 C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? C12 C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? O2 C16 Cr 176.2(2) . . ? O3 C17 Cr 176.6(2) . . ? O4 C18 Cr 174.3(2) . . ? O5 C19 Cr 173.4(2) . . ? O6 C20 Cr 174.7(2) . . ? C16 Cr C18 85.33(11) . . ? C16 Cr C17 86.96(10) . . ? C18 Cr C17 95.50(11) . . ? C16 Cr C19 89.81(10) . . ? C18 Cr C19 88.32(11) . . ? C17 Cr C19 174.78(10) . . ? C16 Cr C20 89.25(10) . . ? C18 Cr C20 173.12(11) . . ? C17 Cr C20 88.43(11) . . ? C19 Cr C20 87.42(11) . . ? C16 Cr P 173.10(8) . . ? C18 Cr P 91.53(7) . . ? C17 Cr P 87.22(7) . . ? C19 Cr P 96.25(7) . . ? C20 Cr P 94.31(7) . . ? C11 O1 P 69.06(12) . . ? O1 P C11 50.51(10) . . ? O1 P C1 103.47(10) . . ? C11 P C1 105.18(10) . . ? O1 P Cr 120.81(6) . . ? C11 P Cr 131.77(8) . . ? C1 P Cr 121.61(8) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.617 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.108 #------------------------------------------------------------------------------ data_Greg846 _database_code_depnum_ccdc_archive 'CCDC 792189' #TrackingRef 'Gesamtcif.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H27 Cr O6 P Si2' _chemical_formula_sum 'C16 H27 Cr O6 P Si2' _chemical_formula_weight 454.53 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' Cr Cr 0.3209 0.6236 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2872(3) _cell_length_b 18.4261(8) _cell_length_c 13.4718(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.258(2) _cell_angle_gamma 90.00 _cell_volume 2304.83(14) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6109 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 30.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.695 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.67589 _exptl_absorpt_correction_T_max 0.87597 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19956 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5532 _reflns_number_gt 4030 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5532 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.946 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.68803(18) 0.19881(10) 0.61934(12) 0.0219(4) Uani 1 1 d . . . H1A H 0.7472 0.2427 0.6047 0.026 Uiso 1 1 calc R . . C2 C 0.75331(19) 0.12839(10) 0.58688(13) 0.0263(4) Uani 1 1 d . . . H2A H 0.6966 0.0876 0.6154 0.032 Uiso 1 1 calc R . . C3 C 0.9082(2) 0.12286(11) 0.62584(14) 0.0315(5) Uani 1 1 d . . . H3A H 0.9090 0.1209 0.6985 0.047 Uiso 1 1 calc R . . H3B H 0.9626 0.1654 0.6042 0.047 Uiso 1 1 calc R . . H3C H 0.9525 0.0787 0.5998 0.047 Uiso 1 1 calc R . . C4 C 0.7445(2) 0.12317(12) 0.47348(14) 0.0402(5) Uani 1 1 d . . . H4C H 0.7832 0.0763 0.4523 0.060 Uiso 1 1 calc R . . H4B H 0.8008 0.1625 0.4445 0.060 Uiso 1 1 calc R . . H4A H 0.6438 0.1273 0.4510 0.060 Uiso 1 1 calc R . . C5 C 0.56774(17) 0.30424(9) 0.75692(12) 0.0182(4) Uani 1 1 d . . . H5A H 0.5026 0.3044 0.8150 0.022 Uiso 1 1 calc R . . C6 C 0.84629(19) 0.25539(11) 0.86883(14) 0.0305(4) Uani 1 1 d . . . H6A H 0.8739 0.2222 0.8157 0.046 Uiso 1 1 calc R . . H6B H 0.7837 0.2300 0.9150 0.046 Uiso 1 1 calc R . . H6C H 0.9329 0.2724 0.9045 0.046 Uiso 1 1 calc R . . C7 C 0.7114(2) 0.39976(12) 0.91649(15) 0.0391(5) Uani 1 1 d . . . H7A H 0.6527 0.3760 0.9665 0.059 Uiso 1 1 calc R . . H7B H 0.6595 0.4419 0.8895 0.059 Uiso 1 1 calc R . . H7C H 0.8027 0.4156 0.9472 0.059 Uiso 1 1 calc R . . C8 C 0.8668(2) 0.37837(11) 0.72201(14) 0.0320(5) Uani 1 1 d . . . H8A H 0.8198 0.4222 0.6957 0.048 Uiso 1 1 calc R . . H8B H 0.8844 0.3445 0.6675 0.048 Uiso 1 1 calc R . . H8C H 0.9587 0.3915 0.7544 0.048 Uiso 1 1 calc R . . C9 C 0.28589(19) 0.33052(11) 0.64223(15) 0.0331(5) Uani 1 1 d . . . H9A H 0.2370 0.3259 0.7056 0.050 Uiso 1 1 calc R . . H9B H 0.2921 0.2827 0.6107 0.050 Uiso 1 1 calc R . . H9C H 0.2313 0.3636 0.5986 0.050 Uiso 1 1 calc R . . C10 C 0.4534(2) 0.45777(10) 0.72528(14) 0.0315(4) Uani 1 1 d . . . H10A H 0.5495 0.4771 0.7411 0.047 Uiso 1 1 calc R . . H10B H 0.3993 0.4526 0.7865 0.047 Uiso 1 1 calc R . . H10C H 0.4023 0.4911 0.6801 0.047 Uiso 1 1 calc R . . C11 C 0.5653(2) 0.37853(11) 0.54494(13) 0.0321(5) Uani 1 1 d . . . H11C H 0.5103 0.4117 0.5018 0.048 Uiso 1 1 calc R . . H11B H 0.5736 0.3313 0.5122 0.048 Uiso 1 1 calc R . . H11A H 0.6617 0.3985 0.5579 0.048 Uiso 1 1 calc R . . C12 C 0.39398(19) 0.04620(11) 0.89694(13) 0.0271(4) Uani 1 1 d . . . C13 C 0.48671(18) 0.18001(10) 0.93039(13) 0.0224(4) Uani 1 1 d . . . C14 C 0.2827(2) 0.15921(11) 0.79466(14) 0.0310(5) Uani 1 1 d . . . C15 C 0.4429(2) 0.06011(11) 0.70323(14) 0.0282(4) Uani 1 1 d . . . C16 C 0.6583(2) 0.08349(10) 0.84353(12) 0.0225(4) Uani 1 1 d . . . Cr Cr 0.46984(3) 0.119935(16) 0.817712(19) 0.01946(8) Uani 1 1 d . . . O1 O 0.53127(12) 0.20726(7) 0.59690(8) 0.0226(3) Uani 1 1 d . . . O2 O 0.34864(14) 0.00075(8) 0.94555(10) 0.0377(4) Uani 1 1 d . . . O3 O 0.49261(14) 0.21660(8) 0.99880(9) 0.0344(3) Uani 1 1 d . . . O4 O 0.17008(15) 0.18239(9) 0.78364(12) 0.0521(4) Uani 1 1 d . . . O5 O 0.42383(17) 0.02382(8) 0.63562(10) 0.0444(4) Uani 1 1 d . . . O6 O 0.77161(13) 0.06219(7) 0.86057(9) 0.0316(3) Uani 1 1 d . . . P P 0.56607(4) 0.21001(2) 0.71869(3) 0.01732(11) Uani 1 1 d . . . Si1 Si 0.74815(5) 0.33445(3) 0.81410(3) 0.02096(12) Uani 1 1 d . . . Si2 Si 0.47084(5) 0.36728(3) 0.66458(4) 0.02224(12) Uani 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 C1 0.0237(9) 0.0203(10) 0.0217(9) -0.0008(7) 0.0013(7) -0.0031(7) C2 0.0304(10) 0.0185(10) 0.0303(10) -0.0035(8) 0.0096(8) -0.0017(8) C3 0.0337(11) 0.0257(12) 0.0356(11) 0.0038(9) 0.0124(9) 0.0052(9) C4 0.0471(13) 0.0395(14) 0.0345(11) -0.0144(10) 0.0098(10) -0.0021(10) C5 0.0178(8) 0.0168(9) 0.0200(8) -0.0013(7) 0.0022(7) -0.0006(7) C6 0.0272(10) 0.0320(12) 0.0318(10) 0.0013(9) -0.0104(8) -0.0023(9) C7 0.0373(11) 0.0420(14) 0.0380(11) -0.0191(10) -0.0012(9) -0.0017(10) C8 0.0252(10) 0.0314(12) 0.0393(11) 0.0004(9) 0.0006(9) -0.0066(9) C9 0.0249(10) 0.0277(12) 0.0463(12) 0.0032(9) -0.0093(9) 0.0001(8) C10 0.0345(11) 0.0211(11) 0.0388(11) 0.0021(9) 0.0006(9) 0.0037(9) C11 0.0402(11) 0.0289(12) 0.0269(10) 0.0056(8) -0.0048(9) -0.0033(9) C12 0.0246(9) 0.0278(11) 0.0288(10) 0.0006(8) -0.0011(8) -0.0029(8) C13 0.0208(9) 0.0211(11) 0.0254(9) 0.0062(8) 0.0019(8) 0.0027(7) C14 0.0258(10) 0.0323(12) 0.0349(11) 0.0058(9) 0.0005(9) -0.0060(9) C15 0.0322(10) 0.0218(11) 0.0303(10) 0.0053(8) -0.0029(8) -0.0075(8) C16 0.0291(10) 0.0193(10) 0.0193(9) -0.0002(7) 0.0053(8) -0.0036(8) Cr 0.01872(14) 0.01794(17) 0.02175(15) 0.00135(11) 0.00106(11) -0.00248(12) O1 0.0254(6) 0.0225(7) 0.0197(6) -0.0006(5) -0.0030(5) -0.0009(5) O2 0.0399(8) 0.0339(9) 0.0394(8) 0.0122(7) 0.0012(7) -0.0124(7) O3 0.0412(8) 0.0349(9) 0.0272(7) -0.0061(6) 0.0030(6) 0.0065(7) O4 0.0219(8) 0.0638(12) 0.0707(11) 0.0175(9) -0.0009(7) 0.0047(8) O5 0.0602(10) 0.0365(10) 0.0363(8) -0.0096(7) -0.0053(7) -0.0145(8) O6 0.0250(7) 0.0313(8) 0.0387(8) 0.0039(6) 0.0040(6) 0.0056(6) P 0.0173(2) 0.0165(3) 0.0181(2) -0.00012(18) -0.00047(17) -0.00076(18) Si1 0.0200(2) 0.0201(3) 0.0227(2) -0.0033(2) -0.0012(2) -0.0019(2) Si2 0.0215(2) 0.0186(3) 0.0265(3) 0.0025(2) -0.0029(2) 0.0001(2) _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. ; 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 C1 O1 1.489(2) . ? C1 C2 1.501(2) . ? C1 P 1.7842(16) . ? C1 H1A 1.0000 . ? C2 C3 1.524(3) . ? C2 C4 1.531(2) . ? C2 H2A 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4C 0.9800 . ? C4 H4B 0.9800 . ? C4 H4A 0.9800 . ? C5 P 1.8110(17) . ? C5 Si1 1.9115(17) . ? C5 Si2 1.9125(18) . ? C5 H5A 1.0000 . ? C6 Si1 1.862(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 Si1 1.8676(19) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 Si1 1.8623(18) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 Si2 1.8648(18) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 Si2 1.8657(19) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si2 1.8635(18) . ? C11 H11C 0.9800 . ? C11 H11B 0.9800 . ? C11 H11A 0.9800 . ? C12 O2 1.149(2) . ? C12 Cr 1.8747(19) . ? C13 O3 1.142(2) . ? C13 Cr 1.8825(19) . ? C14 O4 1.137(2) . ? C14 Cr 1.902(2) . ? C15 O5 1.141(2) . ? C15 Cr 1.908(2) . ? C16 O6 1.142(2) . ? C16 Cr 1.8997(19) . ? Cr P 2.3207(5) . ? O1 P 1.6661(12) . ? 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 O1 C1 C2 115.51(14) . . ? O1 C1 P 60.40(7) . . ? C2 C1 P 125.84(13) . . ? O1 C1 H1A 114.5 . . ? C2 C1 H1A 114.5 . . ? P C1 H1A 114.5 . . ? C1 C2 C3 109.98(15) . . ? C1 C2 C4 109.38(16) . . ? C3 C2 C4 111.65(15) . . ? C1 C2 H2A 108.6 . . ? C3 C2 H2A 108.6 . . ? C4 C2 H2A 108.6 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4C 109.5 . . ? C2 C4 H4B 109.5 . . ? H4C C4 H4B 109.5 . . ? C2 C4 H4A 109.5 . . ? H4C C4 H4A 109.5 . . ? H4B C4 H4A 109.5 . . ? P C5 Si1 113.31(9) . . ? P C5 Si2 113.35(9) . . ? Si1 C5 Si2 118.75(9) . . ? P C5 H5A 102.9 . . ? Si1 C5 H5A 102.9 . . ? Si2 C5 H5A 102.9 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C11 H11C 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11C C11 H11B 109.5 . . ? Si2 C11 H11A 109.5 . . ? H11C C11 H11A 109.5 . . ? H11B C11 H11A 109.5 . . ? O2 C12 Cr 179.41(18) . . ? O3 C13 Cr 177.97(15) . . ? O4 C14 Cr 178.06(17) . . ? O5 C15 Cr 178.42(17) . . ? O6 C16 Cr 178.83(16) . . ? C12 Cr C13 89.58(8) . . ? C12 Cr C16 89.77(8) . . ? C13 Cr C16 90.01(7) . . ? C12 Cr C14 90.87(8) . . ? C13 Cr C14 88.14(8) . . ? C16 Cr C14 178.04(8) . . ? C12 Cr C15 89.84(8) . . ? C13 Cr C15 177.19(8) . . ? C16 Cr C15 92.73(8) . . ? C14 Cr C15 89.13(8) . . ? C12 Cr P 179.17(6) . . ? C13 Cr P 90.95(5) . . ? C16 Cr P 89.61(5) . . ? C14 Cr P 89.77(6) . . ? C15 Cr P 89.65(5) . . ? C1 O1 P 68.62(8) . . ? O1 P C1 50.98(7) . . ? O1 P C5 108.03(7) . . ? C1 P C5 108.82(8) . . ? O1 P Cr 118.39(5) . . ? C1 P Cr 127.39(6) . . ? C5 P Cr 121.55(5) . . ? C6 Si1 C8 108.18(9) . . ? C6 Si1 C7 107.90(9) . . ? C8 Si1 C7 109.42(10) . . ? C6 Si1 C5 110.41(8) . . ? C8 Si1 C5 112.61(8) . . ? C7 Si1 C5 108.21(8) . . ? C11 Si2 C9 110.50(9) . . ? C11 Si2 C10 109.08(9) . . ? C9 Si2 C10 107.87(9) . . ? C11 Si2 C5 113.98(8) . . ? C9 Si2 C5 107.64(8) . . ? C10 Si2 C5 107.57(8) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.349 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.069 #------------------------------------------------------------------------------ data_Greg820 _database_code_depnum_ccdc_archive 'CCDC 792190' #TrackingRef 'Gesamtcif.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H25 Cr O6 P Si2' _chemical_formula_sum 'C19 H25 Cr O6 P Si2' _chemical_formula_weight 488.54 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' Cr Cr 0.3209 0.6236 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8967(6) _cell_length_b 10.5532(6) _cell_length_c 13.9398(9) _cell_angle_alpha 86.974(5) _cell_angle_beta 88.606(5) _cell_angle_gamma 67.430(5) _cell_volume 1206.85(13) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4512 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 27.77 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 0.669 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.91912 _exptl_absorpt_correction_T_max 0.96483 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 45 _diffrn_source_power 2.25 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 115 frames, detector distance = 100 mm ; _diffrn_reflns_number 11847 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.1116 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5180 _reflns_number_gt 2703 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5180 _refine_ls_number_parameters 268 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1181 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1500 _refine_ls_wR_factor_gt 0.1319 _refine_ls_goodness_of_fit_ref 0.854 _refine_ls_restrained_S_all 0.858 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7778(6) 0.5196(5) 0.8587(3) 0.0449(12) Uani 1 1 d . . . H1A H 0.8578 0.4236 0.8720 0.054 Uiso 1 1 calc R . . C2 C 0.8264(6) 0.6289(4) 0.8950(3) 0.0403(11) Uani 1 1 d . . . C3 C 0.7214(7) 0.7294(5) 0.9510(3) 0.0497(13) Uani 1 1 d . . . H3A H 0.6170 0.7294 0.9672 0.060 Uiso 1 1 calc R . . C4 C 0.7680(8) 0.8299(5) 0.9833(4) 0.0596(15) Uani 1 1 d . . . H4A H 0.6948 0.8989 1.0218 0.072 Uiso 1 1 calc R . . C5 C 0.9150(8) 0.8321(5) 0.9614(4) 0.0597(16) Uani 1 1 d . . . H5A H 0.9454 0.9024 0.9838 0.072 Uiso 1 1 calc R . . C6 C 1.0211(8) 0.7311(7) 0.9062(5) 0.0733(17) Uani 1 1 d U . . H6A H 1.1253 0.7317 0.8902 0.088 Uiso 1 1 calc R . . C7 C 0.9763(7) 0.6281(6) 0.8736(4) 0.0621(15) Uani 1 1 d U . . H7A H 1.0504 0.5576 0.8365 0.075 Uiso 1 1 calc R . . C8 C 0.6858(5) 0.3744(4) 0.7135(3) 0.0354(10) Uani 1 1 d . . . H8A H 0.6183 0.3963 0.6540 0.043 Uiso 1 1 calc R . . C9 C 0.6883(7) 0.2183(6) 0.9119(4) 0.0573(14) Uani 1 1 d . . . H9A H 0.6614 0.2992 0.9504 0.086 Uiso 1 1 calc R . . H9B H 0.8067 0.1748 0.9039 0.086 Uiso 1 1 calc R . . H9C H 0.6481 0.1529 0.9444 0.086 Uiso 1 1 calc R . . C10 C 0.6180(11) 0.1107(7) 0.7303(5) 0.092(2) Uani 1 1 d . . . H10A H 0.7342 0.0563 0.7211 0.138 Uiso 1 1 calc R . . H10B H 0.5642 0.1356 0.6676 0.138 Uiso 1 1 calc R . . H10C H 0.5690 0.0565 0.7693 0.138 Uiso 1 1 calc R . . C11 C 0.3715(7) 0.3729(7) 0.8038(4) 0.0695(17) Uani 1 1 d . . . H11A H 0.3238 0.3986 0.7396 0.104 Uiso 1 1 calc R . . H11B H 0.3540 0.4562 0.8381 0.104 Uiso 1 1 calc R . . H11C H 0.3195 0.3180 0.8394 0.104 Uiso 1 1 calc R . . C12 C 0.9889(7) 0.4076(6) 0.6243(4) 0.0663(16) Uani 1 1 d . . . H12A H 0.9850 0.4671 0.6767 0.099 Uiso 1 1 calc R . . H12B H 0.9256 0.4635 0.5698 0.099 Uiso 1 1 calc R . . H12C H 1.1021 0.3594 0.6042 0.099 Uiso 1 1 calc R . . C13 C 1.0403(7) 0.1634(5) 0.7585(4) 0.0570(14) Uani 1 1 d . . . H13A H 0.9979 0.0945 0.7825 0.086 Uiso 1 1 calc R . . H13B H 1.0487 0.2172 0.8118 0.086 Uiso 1 1 calc R . . H13C H 1.1481 0.1173 0.7299 0.086 Uiso 1 1 calc R . . C14 C 0.8872(8) 0.1810(7) 0.5640(4) 0.083(2) Uani 1 1 d . . . H14C H 0.9931 0.1441 0.5316 0.125 Uiso 1 1 calc R . . H14B H 0.8052 0.2416 0.5188 0.125 Uiso 1 1 calc R . . H14A H 0.8560 0.1051 0.5870 0.125 Uiso 1 1 calc R . . C15 C 0.4077(6) 0.9059(5) 0.5932(3) 0.0447(12) Uani 1 1 d . . . C16 C 0.4441(7) 0.8388(5) 0.7771(4) 0.0514(13) Uani 1 1 d . . . C17 C 0.7141(7) 0.7748(5) 0.6566(4) 0.0487(13) Uani 1 1 d . . . C18 C 0.5764(6) 0.6476(5) 0.5478(3) 0.0433(11) Uani 1 1 d . . . C19 C 0.3295(7) 0.6990(5) 0.6701(3) 0.0493(12) Uani 1 1 d . . . Cr Cr 0.51835(9) 0.74142(7) 0.66381(5) 0.0374(2) Uani 1 1 d . . . O1 O 0.6039(4) 0.5391(3) 0.8736(2) 0.0458(8) Uani 1 1 d . . . O2 O 0.3380(5) 1.0090(3) 0.5515(2) 0.0555(9) Uani 1 1 d . . . O3 O 0.3887(6) 0.9016(4) 0.8429(3) 0.0718(12) Uani 1 1 d . . . O4 O 0.8308(5) 0.7940(4) 0.6488(3) 0.0663(11) Uani 1 1 d . . . O5 O 0.6069(5) 0.5946(4) 0.4764(2) 0.0555(9) Uani 1 1 d . . . O6 O 0.2130(5) 0.6764(4) 0.6745(3) 0.0723(12) Uani 1 1 d . . . P P 0.65101(16) 0.54155(11) 0.75611(8) 0.0395(3) Uani 1 1 d . . . Si1 Si 0.5921(2) 0.27120(15) 0.79310(11) 0.0536(4) Uani 1 1 d . . . Si2 Si 0.90064(17) 0.27891(14) 0.66661(9) 0.0465(4) Uani 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 C1 0.052(3) 0.034(2) 0.047(3) -0.0052(19) -0.013(2) -0.013(2) C2 0.046(3) 0.039(2) 0.036(2) -0.0033(18) -0.013(2) -0.016(2) C3 0.057(3) 0.057(3) 0.041(3) -0.013(2) -0.002(2) -0.027(3) C4 0.069(4) 0.049(3) 0.061(3) -0.020(2) -0.010(3) -0.020(3) C5 0.081(4) 0.048(3) 0.061(3) 0.003(2) -0.030(3) -0.036(3) C6 0.071(3) 0.089(3) 0.077(3) -0.016(3) -0.007(3) -0.047(3) C7 0.055(3) 0.070(3) 0.067(3) -0.025(2) -0.006(2) -0.027(2) C8 0.037(2) 0.035(2) 0.036(2) -0.0050(17) -0.0086(18) -0.0149(19) C9 0.057(3) 0.056(3) 0.062(3) 0.015(2) -0.007(3) -0.027(3) C10 0.128(7) 0.073(4) 0.099(5) -0.015(4) -0.008(5) -0.064(5) C11 0.055(4) 0.090(4) 0.071(4) 0.012(3) -0.010(3) -0.038(3) C12 0.044(3) 0.083(4) 0.066(4) -0.001(3) 0.005(3) -0.018(3) C13 0.051(3) 0.054(3) 0.053(3) -0.009(2) -0.006(2) -0.004(3) C14 0.067(4) 0.092(5) 0.064(4) -0.036(3) -0.015(3) 0.003(3) C15 0.044(3) 0.047(3) 0.044(3) -0.003(2) -0.005(2) -0.017(2) C16 0.063(4) 0.038(3) 0.046(3) 0.003(2) -0.012(3) -0.011(2) C17 0.054(3) 0.033(2) 0.059(3) -0.001(2) -0.018(3) -0.017(2) C18 0.039(3) 0.045(3) 0.049(3) 0.001(2) -0.010(2) -0.018(2) C19 0.047(3) 0.054(3) 0.044(3) 0.003(2) -0.008(2) -0.015(3) Cr 0.0417(4) 0.0321(4) 0.0355(4) -0.0028(3) -0.0097(3) -0.0102(3) O1 0.048(2) 0.0468(18) 0.0441(18) -0.0073(14) -0.0020(15) -0.0197(16) O2 0.058(2) 0.0446(19) 0.055(2) 0.0126(16) -0.0096(18) -0.0109(17) O3 0.094(3) 0.054(2) 0.047(2) -0.0097(18) -0.005(2) -0.004(2) O4 0.054(3) 0.054(2) 0.097(3) 0.003(2) -0.016(2) -0.027(2) O5 0.062(2) 0.064(2) 0.0420(19) -0.0170(16) -0.0025(17) -0.0233(19) O6 0.053(3) 0.085(3) 0.081(3) 0.010(2) -0.009(2) -0.030(2) P 0.0464(7) 0.0317(6) 0.0399(6) -0.0044(5) -0.0140(5) -0.0134(5) Si1 0.0552(9) 0.0533(8) 0.0600(9) 0.0045(7) -0.0100(7) -0.0297(7) Si2 0.0420(8) 0.0495(7) 0.0388(7) -0.0095(6) -0.0057(6) -0.0059(6) _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. ; 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 C1 O1 1.491(6) . ? C1 C2 1.493(6) . ? C1 P 1.793(4) . ? C1 H1A 1.0000 . ? C2 C7 1.356(8) . ? C2 C3 1.378(7) . ? C3 C4 1.377(7) . ? C3 H3A 0.9500 . ? C4 C5 1.345(9) . ? C4 H4A 0.9500 . ? C5 C6 1.378(9) . ? C5 H5A 0.9500 . ? C6 C7 1.393(8) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 P 1.800(4) . ? C8 Si2 1.904(5) . ? C8 Si1 1.907(5) . ? C8 H8A 1.0000 . ? C9 Si1 1.841(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 Si1 1.881(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si1 1.848(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Si2 1.876(7) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 Si2 1.849(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 Si2 1.841(5) . ? C14 H14C 0.9800 . ? C14 H14B 0.9800 . ? C14 H14A 0.9800 . ? C15 O2 1.157(5) . ? C15 Cr 1.873(5) . ? C16 O3 1.146(6) . ? C16 Cr 1.894(5) . ? C17 O4 1.133(6) . ? C17 Cr 1.904(6) . ? C18 O5 1.142(5) . ? C18 Cr 1.897(5) . ? C19 O6 1.149(6) . ? C19 Cr 1.896(6) . ? Cr P 2.3181(13) . ? O1 P 1.682(3) . ? 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 O1 C1 C2 116.0(4) . . ? O1 C1 P 60.8(2) . . ? C2 C1 P 124.5(3) . . ? O1 C1 H1A 114.8 . . ? C2 C1 H1A 114.8 . . ? P C1 H1A 114.8 . . ? C7 C2 C3 119.8(4) . . ? C7 C2 C1 119.6(4) . . ? C3 C2 C1 120.6(5) . . ? C4 C3 C2 119.8(5) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C5 C4 C3 121.2(5) . . ? C5 C4 H4A 119.4 . . ? C3 C4 H4A 119.4 . . ? C4 C5 C6 119.1(5) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? C5 C6 C7 120.3(6) . . ? C5 C6 H6A 119.9 . . ? C7 C6 H6A 119.9 . . ? C2 C7 C6 119.7(6) . . ? C2 C7 H7A 120.1 . . ? C6 C7 H7A 120.1 . . ? P C8 Si2 114.2(2) . . ? P C8 Si1 113.9(2) . . ? Si2 C8 Si1 117.1(2) . . ? P C8 H8A 103.1 . . ? Si2 C8 H8A 103.1 . . ? Si1 C8 H8A 103.1 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C14 H14C 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? Si2 C14 H14A 109.5 . . ? H14C C14 H14A 109.5 . . ? H14B C14 H14A 109.5 . . ? O2 C15 Cr 178.4(4) . . ? O3 C16 Cr 175.2(5) . . ? O4 C17 Cr 177.5(5) . . ? O5 C18 Cr 177.6(4) . . ? O6 C19 Cr 178.4(5) . . ? C15 Cr C16 88.1(2) . . ? C15 Cr C19 91.5(2) . . ? C16 Cr C19 87.8(2) . . ? C15 Cr C18 89.8(2) . . ? C16 Cr C18 175.8(2) . . ? C19 Cr C18 88.7(2) . . ? C15 Cr C17 90.7(2) . . ? C16 Cr C17 94.1(2) . . ? C19 Cr C17 177.2(2) . . ? C18 Cr C17 89.6(2) . . ? C15 Cr P 177.98(16) . . ? C16 Cr P 89.95(14) . . ? C19 Cr P 88.15(15) . . ? C18 Cr P 92.17(14) . . ? C17 Cr P 89.74(14) . . ? C1 O1 P 68.5(2) . . ? O1 P C1 50.7(2) . . ? O1 P C8 107.47(19) . . ? C1 P C8 108.3(2) . . ? O1 P Cr 118.24(12) . . ? C1 P Cr 127.73(15) . . ? C8 P Cr 121.98(14) . . ? C9 Si1 C11 111.5(3) . . ? C9 Si1 C10 107.6(3) . . ? C11 Si1 C10 107.6(3) . . ? C9 Si1 C8 113.7(2) . . ? C11 Si1 C8 108.3(2) . . ? C10 Si1 C8 107.9(3) . . ? C14 Si2 C13 110.3(3) . . ? C14 Si2 C12 109.0(3) . . ? C13 Si2 C12 107.1(3) . . ? C14 Si2 C8 108.0(3) . . ? C13 Si2 C8 113.5(2) . . ? C12 Si2 C8 108.8(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.154 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.074 #------------------------------------------------------------------------------ data_Greg1162 _database_code_depnum_ccdc_archive 'CCDC 792191' #TrackingRef 'Gesamtcif.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H27 Mo O6 P Si2' _chemical_formula_sum 'C16 H27 Mo O6 P Si2' _chemical_formula_weight 498.47 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' Mo Mo -1.6832 0.6857 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6685(6) _cell_length_b 11.1803(6) _cell_length_c 22.4540(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.611(3) _cell_angle_gamma 90.00 _cell_volume 2426.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4366 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.88 _exptl_crystal_description plates _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.83463 _exptl_absorpt_correction_T_max 0.91672 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12950 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4708 _reflns_number_gt 3362 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0078P)^2^+5.6230P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0024(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4708 _refine_ls_number_parameters 361 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.1149 _refine_ls_goodness_of_fit_ref 1.210 _refine_ls_restrained_S_all 1.209 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7862(6) 0.2723(5) 0.4700(2) 0.0450(14) Uani 0.634(3) 1 d P A 1 H1A H 0.8681 0.3261 0.4758 0.054 Uiso 0.634(3) 1 calc PR A 1 C1S C 0.7862(6) 0.2723(5) 0.4700(2) 0.0450(14) Uani 0.366(3) 1 d P A 2 H1B H 0.8142 0.3528 0.4854 0.054 Uiso 0.366(3) 1 calc PR A 2 C2S C 0.7735(7) 0.1752(5) 0.5154(2) 0.0492(15) Uani 0.366(3) 1 d P A 2 H2S H 0.7008 0.1168 0.5020 0.059 Uiso 0.366(3) 1 calc PR A 2 C2 C 0.7735(7) 0.1752(5) 0.5154(2) 0.0492(15) Uani 0.634(3) 1 d P A 1 H2 H 0.7344 0.1025 0.4952 0.059 Uiso 0.634(3) 1 calc PR A 1 C3S C 0.919(2) 0.113(2) 0.5168(10) 0.072(4) Uani 0.366(3) 1 d PU A 2 H3D H 0.9909 0.1726 0.5261 0.109 Uiso 0.366(3) 1 calc PR A 2 H3E H 0.9358 0.0772 0.4779 0.109 Uiso 0.366(3) 1 calc PR A 2 H3F H 0.9214 0.0506 0.5474 0.109 Uiso 0.366(3) 1 calc PR A 2 C3 C 0.9064(14) 0.1432(12) 0.5444(6) 0.076(3) Uani 0.634(3) 1 d PU A 1 H3A H 0.9443 0.2128 0.5658 0.114 Uiso 0.634(3) 1 calc PR A 1 H3B H 0.9714 0.1176 0.5142 0.114 Uiso 0.634(3) 1 calc PR A 1 H3C H 0.8923 0.0778 0.5726 0.114 Uiso 0.634(3) 1 calc PR A 1 C4S C 0.743(2) 0.220(2) 0.5759(9) 0.064(3) Uani 0.366(3) 1 d PU A 2 H4D H 0.6489 0.2517 0.5762 0.095 Uiso 0.366(3) 1 calc PR A 2 H4E H 0.8091 0.2834 0.5870 0.095 Uiso 0.366(3) 1 calc PR A 2 H4F H 0.7522 0.1541 0.6046 0.095 Uiso 0.366(3) 1 calc PR A 2 C4 C 0.6698(12) 0.2188(11) 0.5622(5) 0.061(3) Uani 0.634(3) 1 d PU A 1 H4A H 0.5777 0.2271 0.5433 0.092 Uiso 0.634(3) 1 calc PR A 1 H4B H 0.7002 0.2963 0.5782 0.092 Uiso 0.634(3) 1 calc PR A 1 H4C H 0.6660 0.1604 0.5946 0.092 Uiso 0.634(3) 1 calc PR A 1 C5 C 0.7906(11) 0.3841(11) 0.3513(6) 0.032(3) Uani 0.634(3) 1 d P A 1 H5A H 0.7447 0.3712 0.3114 0.038 Uiso 0.634(3) 1 calc PR A 1 C5S C 0.7401(19) 0.4085(18) 0.3650(9) 0.026(4) Uani 0.366(3) 1 d P A 2 H5B H 0.6925 0.4006 0.3251 0.031 Uiso 0.366(3) 1 calc PR A 2 C6 C 1.0258(9) 0.1956(9) 0.3508(4) 0.052(3) Uani 0.634(3) 1 d P A 1 H6A H 0.9693 0.1438 0.3246 0.078 Uiso 0.634(3) 1 calc PR A 1 H6B H 1.0081 0.1763 0.3925 0.078 Uiso 0.634(3) 1 calc PR A 1 H6C H 1.1239 0.1829 0.3430 0.078 Uiso 0.634(3) 1 calc PR A 1 C6S C 1.0415(18) 0.4674(19) 0.4107(9) 0.050(5) Uani 0.366(3) 1 d P A 2 H6D H 1.0623 0.3880 0.4272 0.075 Uiso 0.366(3) 1 calc PR A 2 H6E H 0.9983 0.5166 0.4411 0.075 Uiso 0.366(3) 1 calc PR A 2 H6F H 1.1273 0.5055 0.3984 0.075 Uiso 0.366(3) 1 calc PR A 2 C7 C 1.0955(12) 0.4452(11) 0.3845(5) 0.054(3) Uani 0.634(3) 1 d P A 1 H7A H 1.0819 0.4235 0.4262 0.081 Uiso 0.634(3) 1 calc PR A 1 H7B H 1.0742 0.5301 0.3787 0.081 Uiso 0.634(3) 1 calc PR A 1 H7C H 1.1919 0.4302 0.3744 0.081 Uiso 0.634(3) 1 calc PR A 1 C7S C 0.912(2) 0.5991(17) 0.3079(9) 0.066(6) Uani 0.366(3) 1 d P A 2 H7D H 0.8813 0.6596 0.3362 0.099 Uiso 0.366(3) 1 calc PR A 2 H7E H 0.8464 0.5954 0.2739 0.099 Uiso 0.366(3) 1 calc PR A 2 H7F H 1.0038 0.6206 0.2939 0.099 Uiso 0.366(3) 1 calc PR A 2 C8 C 1.0059(12) 0.3921(10) 0.2556(4) 0.050(3) Uani 0.634(3) 1 d P A 1 H8A H 0.9846 0.4768 0.2488 0.076 Uiso 0.634(3) 1 calc PR A 1 H8B H 0.9443 0.3427 0.2305 0.076 Uiso 0.634(3) 1 calc PR A 1 H8C H 1.1023 0.3765 0.2456 0.076 Uiso 0.634(3) 1 calc PR A 1 C8S C 0.9865(17) 0.3460(18) 0.2889(11) 0.062(6) Uani 0.366(3) 1 d P A 2 H8D H 0.9187 0.3384 0.2559 0.093 Uiso 0.366(3) 1 calc PR A 2 H8E H 1.0016 0.2676 0.3075 0.093 Uiso 0.366(3) 1 calc PR A 2 H8F H 1.0740 0.3759 0.2738 0.093 Uiso 0.366(3) 1 calc PR A 2 C9 C 0.5512(14) 0.5550(11) 0.3641(6) 0.067(4) Uani 0.634(3) 1 d P A 1 H9A H 0.5111 0.5126 0.3978 0.101 Uiso 0.634(3) 1 calc PR A 1 H9B H 0.5179 0.5186 0.3267 0.101 Uiso 0.634(3) 1 calc PR A 1 H9C H 0.5234 0.6392 0.3651 0.101 Uiso 0.634(3) 1 calc PR A 1 C9S C 0.561(2) 0.625(2) 0.3470(8) 0.056(5) Uani 0.366(3) 1 d P A 2 H9D H 0.5198 0.5790 0.3140 0.084 Uiso 0.366(3) 1 calc PR A 2 H9E H 0.6364 0.6749 0.3322 0.084 Uiso 0.366(3) 1 calc PR A 2 H9F H 0.4908 0.6762 0.3644 0.084 Uiso 0.366(3) 1 calc PR A 2 C10 C 0.8169(14) 0.6434(9) 0.3124(5) 0.067(3) Uani 0.634(3) 1 d P A 1 H10A H 0.8049 0.6065 0.2730 0.100 Uiso 0.634(3) 1 calc PR A 1 H10B H 0.9157 0.6545 0.3217 0.100 Uiso 0.634(3) 1 calc PR A 1 H10C H 0.7702 0.7212 0.3126 0.100 Uiso 0.634(3) 1 calc PR A 1 C10S C 0.726(2) 0.6024(19) 0.4641(10) 0.055(5) Uani 0.366(3) 1 d P A 2 H10D H 0.8045 0.6452 0.4477 0.083 Uiso 0.366(3) 1 calc PR A 2 H10E H 0.7593 0.5439 0.4936 0.083 Uiso 0.366(3) 1 calc PR A 2 H10F H 0.6641 0.6595 0.4832 0.083 Uiso 0.366(3) 1 calc PR A 2 C11 C 0.8023(13) 0.5956(10) 0.4451(5) 0.055(3) Uani 0.634(3) 1 d P A 1 H11A H 0.9022 0.6105 0.4447 0.082 Uiso 0.634(3) 1 calc PR A 1 H11B H 0.7829 0.5335 0.4746 0.082 Uiso 0.634(3) 1 calc PR A 1 H11C H 0.7542 0.6695 0.4557 0.082 Uiso 0.634(3) 1 calc PR A 1 C11S C 0.4787(18) 0.4509(15) 0.4393(9) 0.066(6) Uani 0.366(3) 1 d P A 2 H11D H 0.5124 0.3887 0.4668 0.099 Uiso 0.366(3) 1 calc PR A 2 H11E H 0.4179 0.4148 0.4086 0.099 Uiso 0.366(3) 1 calc PR A 2 H11F H 0.4271 0.5111 0.4613 0.099 Uiso 0.366(3) 1 calc PR A 2 C12 C 0.4478(6) -0.0139(5) 0.3099(2) 0.0437(14) Uani 1 1 d . . . C13 C 0.4502(6) 0.1085(5) 0.4235(3) 0.0489(14) Uani 1 1 d . . . C14 C 0.6930(7) -0.0204(5) 0.3831(3) 0.0488(15) Uani 1 1 d . . . C15 C 0.6854(6) 0.1193(5) 0.2746(3) 0.0418(13) Uani 1 1 d . . . C16 C 0.4428(5) 0.2415(5) 0.3135(3) 0.0414(13) Uani 1 1 d . . . Mo Mo 0.56782(5) 0.11133(4) 0.34895(2) 0.03508(18) Uani 1 1 d . A . O1 O 0.6460(6) 0.3370(5) 0.4564(2) 0.0431(15) Uani 0.634(3) 1 d P A 1 O1S O 0.8815(10) 0.2157(8) 0.4190(4) 0.041(3) Uani 0.366(3) 1 d P A 2 O2 O 0.3764(4) -0.0866(4) 0.28868(18) 0.0585(12) Uani 1 1 d . . . O3 O 0.3836(5) 0.1069(4) 0.4644(2) 0.0734(14) Uani 1 1 d . . . O4 O 0.7639(5) -0.0955(4) 0.4010(2) 0.0737(14) Uani 1 1 d . . . O5 O 0.7494(4) 0.1254(4) 0.23278(19) 0.0567(11) Uani 1 1 d . . . O6 O 0.3741(4) 0.3139(4) 0.2922(2) 0.0607(12) Uani 1 1 d . . . P P 0.71445(15) 0.26756(12) 0.39625(6) 0.0361(3) Uani 1 1 d . . . Si2 Si 0.7404(3) 0.5446(2) 0.36953(11) 0.0442(8) Uani 0.634(3) 1 d P A 1 Si2S Si 0.6297(4) 0.5238(3) 0.40311(18) 0.0357(12) Uani 0.366(3) 1 d P A 2 Si1 Si 0.9802(3) 0.3546(2) 0.33611(13) 0.0390(7) Uani 0.634(3) 1 d P A 1 Si1S Si 0.9205(4) 0.4521(4) 0.3449(2) 0.0432(13) Uani 0.366(3) 1 d P A 2 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 C1 0.059(4) 0.040(3) 0.036(3) -0.004(2) 0.000(3) -0.013(3) C1S 0.059(4) 0.040(3) 0.036(3) -0.004(2) 0.000(3) -0.013(3) C2S 0.075(4) 0.038(3) 0.035(3) 0.000(3) -0.003(3) -0.008(3) C2 0.075(4) 0.038(3) 0.035(3) 0.000(3) -0.003(3) -0.008(3) C3S 0.078(5) 0.068(5) 0.071(5) 0.008(4) 0.000(4) 0.005(4) C3 0.081(4) 0.069(4) 0.077(5) 0.011(4) -0.003(4) 0.005(3) C4S 0.068(5) 0.062(4) 0.061(4) 0.003(4) 0.006(4) 0.000(4) C4 0.067(4) 0.060(4) 0.058(4) 0.004(3) 0.006(3) -0.004(4) C5 0.043(7) 0.025(5) 0.027(6) -0.005(4) -0.002(5) 0.005(5) C5S 0.030(11) 0.030(11) 0.019(10) -0.002(7) -0.002(7) 0.002(8) C6 0.046(5) 0.069(7) 0.042(6) 0.004(5) 0.002(4) 0.013(5) C6S 0.038(11) 0.067(13) 0.046(13) -0.003(10) 0.000(8) -0.008(9) C7 0.051(7) 0.075(8) 0.036(7) -0.003(6) -0.004(5) -0.010(6) C7S 0.058(12) 0.063(14) 0.077(14) 0.020(11) 0.006(11) -0.009(11) C8 0.062(6) 0.056(7) 0.034(6) 0.009(5) 0.005(5) -0.015(6) C8S 0.031(9) 0.069(14) 0.09(2) -0.014(13) 0.007(11) 0.002(9) C9 0.088(9) 0.047(7) 0.065(9) -0.005(6) -0.012(7) 0.032(7) C9S 0.041(9) 0.089(16) 0.039(10) 0.011(11) -0.001(7) 0.033(12) C10 0.122(11) 0.035(6) 0.043(6) 0.003(4) 0.002(7) 0.003(7) C10S 0.066(13) 0.038(10) 0.061(14) -0.035(10) -0.015(10) -0.002(11) C11 0.087(9) 0.035(6) 0.044(7) -0.004(5) 0.005(6) -0.001(7) C11S 0.068(12) 0.046(10) 0.087(14) -0.014(9) 0.050(11) 0.009(9) C12 0.052(3) 0.047(3) 0.032(3) 0.006(3) -0.001(3) 0.001(3) C13 0.057(4) 0.036(3) 0.054(4) -0.006(3) 0.001(3) -0.012(3) C14 0.065(4) 0.037(3) 0.044(4) -0.008(3) -0.006(3) -0.005(3) C15 0.040(3) 0.038(3) 0.047(4) -0.009(3) -0.007(3) 0.000(3) C16 0.034(3) 0.042(3) 0.048(4) -0.009(3) 0.004(3) -0.006(3) Mo 0.0401(3) 0.0319(3) 0.0331(3) -0.0029(2) -0.00197(18) -0.0031(2) O1 0.058(4) 0.032(3) 0.040(3) -0.008(3) 0.014(3) 0.005(3) O1S 0.047(6) 0.038(6) 0.038(6) 0.000(4) -0.003(5) 0.005(5) O2 0.075(3) 0.058(3) 0.042(2) 0.000(2) -0.010(2) -0.028(2) O3 0.091(3) 0.074(3) 0.057(3) -0.011(3) 0.033(3) -0.025(3) O4 0.097(4) 0.047(3) 0.075(3) 0.002(2) -0.019(3) 0.018(3) O5 0.049(2) 0.075(3) 0.047(3) -0.008(2) 0.010(2) -0.001(2) O6 0.045(2) 0.058(3) 0.079(3) 0.005(2) -0.007(2) 0.013(2) P 0.0436(8) 0.0330(7) 0.0316(8) -0.0032(6) -0.0008(6) -0.0038(7) Si2 0.0678(18) 0.0268(13) 0.0377(15) -0.0026(10) -0.0033(13) 0.0048(12) Si2S 0.045(3) 0.027(2) 0.035(2) -0.0044(17) -0.007(2) 0.0057(19) Si1 0.0413(14) 0.0439(16) 0.0315(15) 0.0011(11) -0.0034(11) -0.0062(12) Si1S 0.038(2) 0.050(3) 0.042(3) 0.000(2) 0.0039(19) -0.004(2) _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. ; 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 C1 O1 1.559(8) . ? C1 P 1.778(6) . ? C1 H1A 1.0000 . ? C2S C4S 1.49(2) . ? C2S C3S 1.57(2) . ? C2S H2S 1.0000 . ? C3S H3D 0.9800 . ? C3S H3E 0.9800 . ? C3S H3F 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4S H4D 0.9800 . ? C4S H4E 0.9800 . ? C4S H4F 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 P 1.816(13) . ? C5 Si1 1.903(11) . ? C5 Si2 1.906(11) . ? C5 H5A 1.0000 . ? C5S P 1.75(2) . ? C5S Si1S 1.879(18) . ? C5S Si2S 1.894(17) . ? C5S H5B 1.0000 . ? C6 Si1 1.859(10) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C6S Si1S 1.866(19) . ? C6S H6D 0.9800 . ? C6S H6E 0.9800 . ? C6S H6F 0.9800 . ? C7 Si1 1.839(11) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C7S Si1S 1.843(19) . ? C7S H7D 0.9800 . ? C7S H7E 0.9800 . ? C7S H7F 0.9800 . ? C8 Si1 1.879(9) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C8S Si1S 1.85(2) . ? C8S H8D 0.9800 . ? C8S H8E 0.9800 . ? C8S H8F 0.9800 . ? C9 Si2 1.834(13) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C9S Si2S 1.804(18) . ? C9S H9D 0.9800 . ? C9S H9E 0.9800 . ? C9S H9F 0.9800 . ? C10 Si2 1.861(11) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10S Si2S 1.854(17) . ? C10S H10D 0.9800 . ? C10S H10E 0.9800 . ? C10S H10F 0.9800 . ? C11 Si2 1.873(12) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11S Si2S 1.876(16) . ? C11S H11D 0.9800 . ? C11S H11E 0.9800 . ? C11S H11F 0.9800 . ? C12 O2 1.161(6) . ? C12 Mo 2.004(6) . ? C13 O3 1.136(7) . ? C13 Mo 2.051(6) . ? C14 O4 1.149(7) . ? C14 Mo 2.042(6) . ? C15 O5 1.142(6) . ? C15 Mo 2.047(6) . ? C16 O6 1.143(6) . ? C16 Mo 2.040(6) . ? Mo P 2.4707(14) . ? O1 P 1.707(5) . ? O1S P 1.777(9) . ? 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 O1 C1 P 61.1(3) . . ? O1 C1 H1A 115.3 . . ? P C1 H1A 115.3 . . ? C4S C2S C3S 109.2(12) . . ? C4S C2S H2S 109.9 . . ? C3S C2S H2S 109.9 . . ? C2S C3S H3D 109.5 . . ? C2S C3S H3E 109.5 . . ? H3D C3S H3E 109.5 . . ? C2S C3S H3F 109.5 . . ? H3D C3S H3F 109.5 . . ? H3E C3S H3F 109.5 . . ? C2S C4S H4D 109.5 . . ? C2S C4S H4E 109.5 . . ? H4D C4S H4E 109.5 . . ? C2S C4S H4F 109.5 . . ? H4D C4S H4F 109.5 . . ? H4E C4S H4F 109.5 . . ? P C5 Si1 112.5(6) . . ? P C5 Si2 116.5(5) . . ? Si1 C5 Si2 117.0(6) . . ? P C5 H5A 102.6 . . ? Si1 C5 H5A 102.6 . . ? Si2 C5 H5A 102.6 . . ? P C5S Si1S 118.3(10) . . ? P C5S Si2S 110.1(9) . . ? Si1S C5S Si2S 118.1(11) . . ? P C5S H5B 102.4 . . ? Si1S C5S H5B 102.4 . . ? Si2S C5S H5B 102.4 . . ? Si1S C6S H6D 109.5 . . ? Si1S C6S H6E 109.5 . . ? H6D C6S H6E 109.5 . . ? Si1S C6S H6F 109.5 . . ? H6D C6S H6F 109.5 . . ? H6E C6S H6F 109.5 . . ? Si1S C7S H7D 109.5 . . ? Si1S C7S H7E 109.5 . . ? H7D C7S H7E 109.5 . . ? Si1S C7S H7F 109.5 . . ? H7D C7S H7F 109.5 . . ? H7E C7S H7F 109.5 . . ? Si1S C8S H8D 109.5 . . ? Si1S C8S H8E 109.5 . . ? H8D C8S H8E 109.5 . . ? Si1S C8S H8F 109.5 . . ? H8D C8S H8F 109.5 . . ? H8E C8S H8F 109.5 . . ? Si2S C9S H9D 109.5 . . ? Si2S C9S H9E 109.5 . . ? H9D C9S H9E 109.5 . . ? Si2S C9S H9F 109.5 . . ? H9D C9S H9F 109.5 . . ? H9E C9S H9F 109.5 . . ? Si2S C10S H10D 109.5 . . ? Si2S C10S H10E 109.5 . . ? H10D C10S H10E 109.5 . . ? Si2S C10S H10F 109.5 . . ? H10D C10S H10F 109.5 . . ? H10E C10S H10F 109.5 . . ? Si2S C11S H11D 109.5 . . ? Si2S C11S H11E 109.5 . . ? H11D C11S H11E 109.5 . . ? Si2S C11S H11F 109.5 . . ? H11D C11S H11F 109.5 . . ? H11E C11S H11F 109.5 . . ? O2 C12 Mo 178.2(5) . . ? O3 C13 Mo 179.1(6) . . ? O4 C14 Mo 178.4(5) . . ? O5 C15 Mo 178.8(5) . . ? O6 C16 Mo 178.2(5) . . ? C12 Mo C16 89.9(2) . . ? C12 Mo C14 89.4(2) . . ? C16 Mo C14 179.0(2) . . ? C12 Mo C15 90.1(2) . . ? C16 Mo C15 89.3(2) . . ? C14 Mo C15 90.0(2) . . ? C12 Mo C13 91.1(2) . . ? C16 Mo C13 89.6(2) . . ? C14 Mo C13 91.1(2) . . ? C15 Mo C13 178.4(2) . . ? C12 Mo P 179.30(16) . . ? C16 Mo P 89.41(15) . . ? C14 Mo P 91.24(16) . . ? C15 Mo P 89.70(15) . . ? C13 Mo P 89.11(16) . . ? C1 O1 P 65.8(3) . . ? O1 P C5S 88.3(6) . . ? O1 P O1S 106.9(4) . . ? C5S P O1S 105.8(7) . . ? O1 P C1 53.1(3) . . ? C5S P C1 107.0(7) . . ? O1S P C1 54.1(4) . . ? O1 P C5 106.6(4) . . ? C5S P C5 20.7(5) . . ? O1S P C5 90.9(5) . . ? C1 P C5 110.0(4) . . ? O1 P Mo 115.5(2) . . ? C5S P Mo 123.5(7) . . ? O1S P Mo 113.5(3) . . ? C1 P Mo 128.72(19) . . ? C5 P Mo 120.3(4) . . ? C9 Si2 C10 109.4(6) . . ? C9 Si2 C11 109.5(6) . . ? C10 Si2 C11 108.7(5) . . ? C9 Si2 C5 107.8(5) . . ? C10 Si2 C5 107.6(5) . . ? C11 Si2 C5 113.8(6) . . ? C9S Si2S C10S 112.6(11) . . ? C9S Si2S C11S 107.5(9) . . ? C10S Si2S C11S 105.4(10) . . ? C9S Si2S C5S 108.2(9) . . ? C10S Si2S C5S 112.3(9) . . ? C11S Si2S C5S 110.8(8) . . ? C7 Si1 C6 106.6(5) . . ? C7 Si1 C8 110.5(5) . . ? C6 Si1 C8 110.3(5) . . ? C7 Si1 C5 111.7(5) . . ? C6 Si1 C5 111.0(5) . . ? C8 Si1 C5 106.8(6) . . ? C7S Si1S C8S 106.1(11) . . ? C7S Si1S C6S 107.1(10) . . ? C8S Si1S C6S 112.0(9) . . ? C7S Si1S C5S 108.0(9) . . ? C8S Si1S C5S 109.7(8) . . ? C6S Si1S C5S 113.5(9) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.476 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.142 #------------------------------------------------------------------------------ data_Greg116 _database_code_depnum_ccdc_archive 'CCDC 792192' #TrackingRef 'Gesamtcif.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H25 Mo O6 P Si2' _chemical_formula_sum 'C19 H25 Mo O6 P Si2' _chemical_formula_weight 532.48 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' Mo Mo -1.6832 0.6857 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8987(2) _cell_length_b 10.6956(3) _cell_length_c 13.9288(5) _cell_angle_alpha 87.1032(12) _cell_angle_beta 88.3077(13) _cell_angle_gamma 68.9673(17) _cell_volume 1235.70(6) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5395 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 29.13 _exptl_crystal_description plate _exptl_crystal_colour 'light yellowish' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 0.722 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.7611 _exptl_absorpt_correction_T_max 0.8691 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18795 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.0970 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 29.11 _reflns_number_total 6450 _reflns_number_gt 4379 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0071P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6450 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0606 _refine_ls_wR_factor_gt 0.0549 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.886 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7809(3) 0.5146(2) 0.86255(16) 0.0261(6) Uani 1 1 d . . . H1A H 0.8611 0.4221 0.8747 0.031 Uiso 1 1 calc R . . C2 C 0.8286(3) 0.6240(2) 0.89625(17) 0.0262(6) Uani 1 1 d . . . C3 C 0.9839(3) 0.6201(3) 0.8793(2) 0.0448(8) Uani 1 1 d . . . H3A H 1.0598 0.5465 0.8479 0.054 Uiso 1 1 calc R . . C4 C 1.0289(4) 0.7229(3) 0.9079(2) 0.0578(9) Uani 1 1 d . . . H4A H 1.1355 0.7202 0.8951 0.069 Uiso 1 1 calc R . . C5 C 0.9222(4) 0.8291(3) 0.9546(2) 0.0507(8) Uani 1 1 d . . . H5A H 0.9541 0.8999 0.9736 0.061 Uiso 1 1 calc R . . C6 C 0.7691(4) 0.8321(3) 0.9735(2) 0.0489(8) Uani 1 1 d . . . H6A H 0.6946 0.9047 1.0066 0.059 Uiso 1 1 calc R . . C7 C 0.7224(3) 0.7295(3) 0.94470(18) 0.0349(6) Uani 1 1 d . . . H7A H 0.6162 0.7320 0.9585 0.042 Uiso 1 1 calc R . . C8 C 0.6876(2) 0.3700(2) 0.71746(16) 0.0219(5) Uani 1 1 d . . . H8A H 0.6217 0.3908 0.6578 0.026 Uiso 1 1 calc R . . C9 C 0.3738(3) 0.3694(3) 0.81006(19) 0.0431(8) Uani 1 1 d . . . H9A H 0.3251 0.3962 0.7466 0.065 Uiso 1 1 calc R . . H9B H 0.3621 0.4497 0.8451 0.065 Uiso 1 1 calc R . . H9C H 0.3198 0.3162 0.8461 0.065 Uiso 1 1 calc R . . C10 C 0.6084(4) 0.1143(3) 0.7312(2) 0.0664(10) Uani 1 1 d . . . H10A H 0.7222 0.0577 0.7247 0.100 Uiso 1 1 calc R . . H10B H 0.5612 0.1403 0.6672 0.100 Uiso 1 1 calc R . . H10C H 0.5509 0.0643 0.7677 0.100 Uiso 1 1 calc R . . C11 C 0.6862(3) 0.2160(3) 0.91499(18) 0.0425(8) Uani 1 1 d . . . H11A H 0.6609 0.2948 0.9540 0.064 Uiso 1 1 calc R . . H11B H 0.8031 0.1746 0.9066 0.064 Uiso 1 1 calc R . . H11C H 0.6449 0.1512 0.9474 0.064 Uiso 1 1 calc R . . C12 C 0.9870(3) 0.4100(3) 0.62566(19) 0.0472(8) Uani 1 1 d . . . H12A H 0.9862 0.4677 0.6782 0.071 Uiso 1 1 calc R . . H12B H 0.9219 0.4645 0.5727 0.071 Uiso 1 1 calc R . . H12C H 1.0979 0.3651 0.6030 0.071 Uiso 1 1 calc R . . C13 C 0.8903(3) 0.1810(3) 0.56729(19) 0.0515(8) Uani 1 1 d . . . H13A H 0.8064 0.2363 0.5231 0.077 Uiso 1 1 calc R . . H13B H 0.8646 0.1033 0.5914 0.077 Uiso 1 1 calc R . . H13C H 0.9943 0.1502 0.5333 0.077 Uiso 1 1 calc R . . C14 C 1.0394(3) 0.1694(3) 0.76187(18) 0.0426(7) Uani 1 1 d . . . H14A H 1.0025 0.0957 0.7812 0.064 Uiso 1 1 calc R . . H14B H 1.0397 0.2207 0.8181 0.064 Uiso 1 1 calc R . . H14C H 1.1486 0.1328 0.7348 0.064 Uiso 1 1 calc R . . C15 C 0.7197(3) 0.7834(2) 0.65888(18) 0.0306(6) Uani 1 1 d . . . C16 C 0.4267(3) 0.8439(2) 0.78547(19) 0.0311(6) Uani 1 1 d . . . C17 C 0.3101(3) 0.6902(2) 0.66874(18) 0.0310(6) Uani 1 1 d . . . C18 C 0.5786(3) 0.6423(2) 0.54016(19) 0.0289(6) Uani 1 1 d . . . C19 C 0.3953(3) 0.9119(3) 0.58732(18) 0.0280(6) Uani 1 1 d . . . Mo Mo 0.51133(2) 0.74017(2) 0.664392(15) 0.02222(7) Uani 1 1 d . . . O1 O 0.61044(17) 0.52898(15) 0.87981(11) 0.0303(4) Uani 1 1 d . . . O2 O 0.83550(19) 0.80574(17) 0.65307(14) 0.0481(5) Uani 1 1 d . . . O3 O 0.3699(2) 0.90601(18) 0.85102(13) 0.0493(5) Uani 1 1 d . . . O4 O 0.19773(19) 0.66209(18) 0.67076(13) 0.0468(5) Uani 1 1 d . . . O5 O 0.6116(2) 0.58903(18) 0.46862(13) 0.0437(5) Uani 1 1 d . . . O6 O 0.32931(19) 1.01075(18) 0.54610(13) 0.0437(5) Uani 1 1 d . . . P P 0.65224(7) 0.53389(6) 0.76168(5) 0.02300(15) Uani 1 1 d . . . Si1 Si 0.59087(8) 0.26755(7) 0.79565(6) 0.03364(19) Uani 1 1 d . . . Si2 Si 0.90121(8) 0.28147(7) 0.66963(5) 0.02947(18) Uani 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 C1 0.0232(12) 0.0242(14) 0.0278(15) -0.0032(11) -0.0043(11) -0.0043(11) C2 0.0312(13) 0.0253(14) 0.0221(14) 0.0007(11) -0.0084(11) -0.0096(11) C3 0.0367(16) 0.055(2) 0.048(2) -0.0183(15) 0.0014(14) -0.0201(15) C4 0.0548(19) 0.075(3) 0.061(2) -0.0146(19) 0.0016(17) -0.0437(19) C5 0.079(2) 0.0414(19) 0.047(2) 0.0026(16) -0.0266(17) -0.0387(18) C6 0.065(2) 0.0332(18) 0.044(2) -0.0111(15) -0.0124(16) -0.0095(15) C7 0.0394(15) 0.0333(16) 0.0321(16) -0.0067(13) -0.0052(13) -0.0121(13) C8 0.0227(12) 0.0182(13) 0.0241(14) -0.0006(10) -0.0061(10) -0.0060(10) C9 0.0337(14) 0.055(2) 0.0472(19) 0.0119(15) -0.0043(13) -0.0251(14) C10 0.086(2) 0.048(2) 0.084(3) -0.0110(18) 0.006(2) -0.0469(19) C11 0.0363(15) 0.0392(17) 0.0498(19) 0.0164(14) -0.0018(14) -0.0132(13) C12 0.0302(14) 0.057(2) 0.051(2) 0.0040(16) 0.0087(14) -0.0130(14) C13 0.0433(16) 0.060(2) 0.0414(19) -0.0192(16) -0.0036(14) -0.0036(15) C14 0.0313(14) 0.0482(19) 0.0379(18) -0.0036(14) -0.0002(13) -0.0013(13) C15 0.0330(14) 0.0197(14) 0.0357(17) 0.0021(12) -0.0054(12) -0.0055(12) C16 0.0364(14) 0.0218(15) 0.0307(16) 0.0053(12) -0.0049(12) -0.0055(12) C17 0.0282(14) 0.0285(15) 0.0304(16) 0.0004(12) 0.0008(12) -0.0033(12) C18 0.0232(13) 0.0296(15) 0.0342(17) 0.0032(13) -0.0035(12) -0.0102(11) C19 0.0265(13) 0.0345(16) 0.0265(15) -0.0031(13) 0.0006(11) -0.0148(12) Mo 0.02294(11) 0.01863(11) 0.02407(13) 0.00019(9) -0.00259(9) -0.00619(9) O1 0.0314(9) 0.0344(10) 0.0273(10) -0.0020(8) 0.0017(8) -0.0147(8) O2 0.0302(10) 0.0410(12) 0.0766(16) 0.0068(11) -0.0074(10) -0.0177(9) O3 0.0637(13) 0.0364(12) 0.0340(12) -0.0058(10) 0.0001(10) -0.0006(10) O4 0.0304(10) 0.0546(14) 0.0582(14) 0.0085(10) -0.0031(10) -0.0200(10) O5 0.0431(11) 0.0548(13) 0.0350(12) -0.0154(10) 0.0043(10) -0.0183(10) O6 0.0416(11) 0.0347(12) 0.0475(13) 0.0137(10) -0.0053(9) -0.0066(9) P 0.0243(3) 0.0210(3) 0.0247(4) -0.0018(3) -0.0014(3) -0.0091(3) Si1 0.0336(4) 0.0287(4) 0.0425(5) 0.0049(4) -0.0022(4) -0.0166(3) Si2 0.0250(4) 0.0314(4) 0.0276(4) -0.0032(3) -0.0024(3) -0.0043(3) _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. ; 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 C1 C2 1.481(3) . ? C1 O1 1.482(2) . ? C1 P 1.795(2) . ? C1 H1A 1.0000 . ? C2 C7 1.377(3) . ? C2 C3 1.382(3) . ? C3 C4 1.377(4) . ? C3 H3A 0.9500 . ? C4 C5 1.371(4) . ? C4 H4A 0.9500 . ? C5 C6 1.369(3) . ? C5 H5A 0.9500 . ? C6 C7 1.385(3) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 P 1.804(2) . ? C8 Si1 1.904(2) . ? C8 Si2 1.911(2) . ? C8 H8A 1.0000 . ? C9 Si1 1.856(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 Si1 1.865(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si1 1.855(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Si2 1.867(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 Si2 1.853(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 Si2 1.865(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 O2 1.139(2) . ? C15 Mo 2.064(2) . ? C16 O3 1.150(3) . ? C16 Mo 2.039(3) . ? C17 O4 1.142(3) . ? C17 Mo 2.043(2) . ? C18 O5 1.151(3) . ? C18 Mo 2.030(3) . ? C19 O6 1.143(3) . ? C19 Mo 2.024(3) . ? Mo P 2.4675(7) . ? O1 P 1.6786(16) . ? 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 C2 C1 O1 116.06(19) . . ? C2 C1 P 123.42(18) . . ? O1 C1 P 60.72(10) . . ? C2 C1 H1A 115.1 . . ? O1 C1 H1A 115.1 . . ? P C1 H1A 115.1 . . ? C7 C2 C3 118.9(2) . . ? C7 C2 C1 121.8(2) . . ? C3 C2 C1 119.3(2) . . ? C4 C3 C2 120.0(3) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C5 C4 C3 121.0(3) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C6 C5 C4 119.3(3) . . ? C6 C5 H5A 120.4 . . ? C4 C5 H5A 120.4 . . ? C5 C6 C7 120.2(3) . . ? C5 C6 H6A 119.9 . . ? C7 C6 H6A 119.9 . . ? C2 C7 C6 120.6(2) . . ? C2 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? P C8 Si1 113.33(11) . . ? P C8 Si2 114.18(11) . . ? Si1 C8 Si2 118.16(11) . . ? P C8 H8A 102.8 . . ? Si1 C8 H8A 102.8 . . ? Si2 C8 H8A 102.8 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 Mo 177.9(2) . . ? O3 C16 Mo 175.8(2) . . ? O4 C17 Mo 179.7(2) . . ? O5 C18 Mo 177.7(2) . . ? O6 C19 Mo 178.1(2) . . ? C19 Mo C18 89.58(9) . . ? C19 Mo C16 87.70(9) . . ? C18 Mo C16 175.74(10) . . ? C19 Mo C17 91.27(9) . . ? C18 Mo C17 88.95(9) . . ? C16 Mo C17 87.84(10) . . ? C19 Mo C15 90.27(9) . . ? C18 Mo C15 89.59(9) . . ? C16 Mo C15 93.70(10) . . ? C17 Mo C15 177.87(9) . . ? C19 Mo P 178.67(7) . . ? C18 Mo P 91.71(7) . . ? C16 Mo P 91.03(7) . . ? C17 Mo P 89.09(7) . . ? C15 Mo P 89.41(7) . . ? C1 O1 P 68.90(10) . . ? O1 P C1 50.37(8) . . ? O1 P C8 107.93(9) . . ? C1 P C8 108.23(11) . . ? O1 P Mo 119.01(6) . . ? C1 P Mo 127.92(8) . . ? C8 P Mo 121.54(8) . . ? C11 Si1 C9 110.31(12) . . ? C11 Si1 C10 108.78(14) . . ? C9 Si1 C10 108.25(13) . . ? C11 Si1 C8 113.07(11) . . ? C9 Si1 C8 107.98(10) . . ? C10 Si1 C8 108.32(11) . . ? C13 Si2 C14 109.14(13) . . ? C13 Si2 C12 108.82(12) . . ? C14 Si2 C12 108.15(12) . . ? C13 Si2 C8 108.24(11) . . ? C14 Si2 C8 113.26(10) . . ? C12 Si2 C8 109.15(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C11 H11A O1 0.98 2.55 3.184(3) 122.4 . C9 H9B O1 0.98 2.70 3.340(3) 123.3 . _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 29.11 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.505 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.091 #------------------------------------------------------------------------------ data_Greg1167 _database_code_depnum_ccdc_archive 'CCDC 792193' #TrackingRef 'Gesamtcif.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H29 Mo O6 P Si2' _chemical_formula_sum 'C17 H29 Mo O6 P Si2' _chemical_formula_weight 512.49 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' Mo Mo -1.6832 0.6857 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5254(2) _cell_length_b 18.8531(7) _cell_length_c 13.6767(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.3656(15) _cell_angle_gamma 90.00 _cell_volume 2455.41(12) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5913 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 29.13 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 0.723 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.6709 _exptl_absorpt_correction_T_max 0.8123 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20039 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5787 _reflns_number_gt 4920 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+0.1667P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5787 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0581 _refine_ls_wR_factor_gt 0.0559 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.14859(14) 0.18413(9) 0.34967(10) 0.0180(3) Uani 1 1 d . . . H1A H -0.2063 0.2284 0.3512 0.022 Uiso 1 1 calc R . . C2 C -0.21674(15) 0.12420(9) 0.40490(10) 0.0218(3) Uani 1 1 d . . . C3 C -0.13205(18) 0.05608(10) 0.40638(13) 0.0334(4) Uani 1 1 d . . . H3A H -0.0401 0.0648 0.4377 0.050 Uiso 1 1 calc R . . H3B H -0.1192 0.0396 0.3392 0.050 Uiso 1 1 calc R . . H3C H -0.1821 0.0198 0.4432 0.050 Uiso 1 1 calc R . . C4 C -0.23369(19) 0.15124(11) 0.51052(11) 0.0340(4) Uani 1 1 d . . . H4C H -0.2807 0.1149 0.5492 0.051 Uiso 1 1 calc R . . H4B H -0.2902 0.1947 0.5096 0.051 Uiso 1 1 calc R . . H4A H -0.1409 0.1613 0.5398 0.051 Uiso 1 1 calc R . . C5 C -0.36236(17) 0.11189(10) 0.35760(13) 0.0333(4) Uani 1 1 d . . . H5A H -0.3519 0.0923 0.2918 0.050 Uiso 1 1 calc R . . H5B H -0.4131 0.1570 0.3533 0.050 Uiso 1 1 calc R . . H5C H -0.4151 0.0784 0.3974 0.050 Uiso 1 1 calc R . . C6 C -0.04742(14) 0.27294(8) 0.19820(10) 0.0158(3) Uani 1 1 d . . . H6A H 0.0230 0.2733 0.1451 0.019 Uiso 1 1 calc R . . C7 C 0.20352(15) 0.33682(10) 0.30865(11) 0.0252(4) Uani 1 1 d . . . H7A H 0.2547 0.3350 0.2474 0.038 Uiso 1 1 calc R . . H7B H 0.2176 0.2923 0.3446 0.038 Uiso 1 1 calc R . . H7C H 0.2386 0.3765 0.3486 0.038 Uiso 1 1 calc R . . C8 C -0.01177(16) 0.43412(9) 0.21127(12) 0.0272(4) Uani 1 1 d . . . H8A H -0.1121 0.4421 0.1979 0.041 Uiso 1 1 calc R . . H8B H 0.0376 0.4310 0.1494 0.041 Uiso 1 1 calc R . . H8C H 0.0265 0.4736 0.2501 0.041 Uiso 1 1 calc R . . C9 C -0.08793(15) 0.35918(9) 0.39583(11) 0.0239(3) Uani 1 1 d . . . H9C H -0.0524 0.4003 0.4327 0.036 Uiso 1 1 calc R . . H9B H -0.0762 0.3163 0.4356 0.036 Uiso 1 1 calc R . . H9A H -0.1877 0.3661 0.3795 0.036 Uiso 1 1 calc R . . C10 C -0.19002(17) 0.33455(11) 0.01454(12) 0.0329(4) Uani 1 1 d . . . H10A H -0.1215 0.3093 -0.0250 0.049 Uiso 1 1 calc R . . H10B H -0.1532 0.3815 0.0319 0.049 Uiso 1 1 calc R . . H10C H -0.2782 0.3398 -0.0231 0.049 Uiso 1 1 calc R . . C11 C -0.35758(15) 0.32924(11) 0.20252(12) 0.0302(4) Uani 1 1 d . . . H11A H -0.3240 0.3768 0.2199 0.045 Uiso 1 1 calc R . . H11B H -0.3739 0.3021 0.2623 0.045 Uiso 1 1 calc R . . H11C H -0.4455 0.3330 0.1642 0.045 Uiso 1 1 calc R . . C12 C -0.29362(16) 0.19458(10) 0.09148(11) 0.0276(4) Uani 1 1 d . . . H12A H -0.3152 0.1671 0.1501 0.041 Uiso 1 1 calc R . . H12B H -0.2236 0.1692 0.0535 0.041 Uiso 1 1 calc R . . H12C H -0.3794 0.2010 0.0515 0.041 Uiso 1 1 calc R . . C13 C 0.24628(18) 0.03244(10) 0.09046(11) 0.0302(4) Uani 1 1 d . . . C14 C 0.28518(16) 0.16565(10) 0.18112(12) 0.0291(4) Uani 1 1 d . . . C15 C 0.06627(15) 0.14659(9) 0.03389(11) 0.0244(4) Uani 1 1 d . . . C16 C -0.04488(19) 0.02848(10) 0.14647(12) 0.0328(4) Uani 1 1 d . . . C17 C 0.17996(16) 0.04908(10) 0.29161(11) 0.0276(4) Uani 1 1 d . . . Mo Mo 0.119027(13) 0.098166(7) 0.163612(8) 0.01848(5) Uani 1 1 d . . . O1 O 0.00124(10) 0.19852(6) 0.37310(7) 0.0196(2) Uani 1 1 d . . . O2 O 0.32017(14) -0.00447(8) 0.05014(9) 0.0465(4) Uani 1 1 d . . . O3 O 0.38010(12) 0.20211(8) 0.18952(11) 0.0488(4) Uani 1 1 d . . . O4 O 0.04043(12) 0.17388(8) -0.03835(8) 0.0388(3) Uani 1 1 d . . . O5 O -0.13444(16) -0.01099(9) 0.13742(10) 0.0578(4) Uani 1 1 d . . . O6 O 0.21725(13) 0.02081(8) 0.36079(9) 0.0442(4) Uani 1 1 d . . . P P -0.02510(4) 0.18597(2) 0.25269(3) 0.01541(9) Uani 1 1 d . . . Si1 Si 0.01220(4) 0.34954(2) 0.28083(3) 0.01810(9) Uani 1 1 d . . . Si2 Si -0.22269(4) 0.28304(3) 0.12841(3) 0.01983(10) Uani 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 C1 0.0176(7) 0.0204(9) 0.0161(7) 0.0003(6) 0.0007(6) 0.0004(6) C2 0.0248(7) 0.0206(9) 0.0202(7) 0.0018(7) 0.0074(6) -0.0012(7) C3 0.0432(10) 0.0239(11) 0.0338(9) 0.0110(8) 0.0166(8) 0.0041(8) C4 0.0444(10) 0.0358(12) 0.0224(8) 0.0017(7) 0.0110(7) -0.0030(9) C5 0.0295(9) 0.0338(12) 0.0368(9) 0.0015(8) 0.0066(7) -0.0116(8) C6 0.0151(6) 0.0173(8) 0.0151(6) 0.0021(6) 0.0018(5) 0.0000(6) C7 0.0204(7) 0.0272(10) 0.0279(8) -0.0050(7) -0.0026(6) -0.0014(7) C8 0.0273(8) 0.0193(9) 0.0352(9) 0.0017(7) 0.0025(7) -0.0008(7) C9 0.0238(7) 0.0233(10) 0.0246(8) -0.0057(7) 0.0022(6) 0.0000(7) C10 0.0299(8) 0.0410(12) 0.0274(8) 0.0134(8) -0.0075(7) -0.0028(8) C11 0.0182(7) 0.0376(12) 0.0347(9) -0.0033(8) -0.0037(7) 0.0044(7) C12 0.0225(8) 0.0352(11) 0.0248(8) -0.0038(7) -0.0031(6) -0.0049(7) C13 0.0429(9) 0.0251(10) 0.0230(8) 0.0073(7) 0.0082(7) 0.0096(8) C14 0.0227(8) 0.0286(11) 0.0364(9) -0.0010(8) 0.0071(7) 0.0052(7) C15 0.0245(8) 0.0260(10) 0.0230(8) -0.0015(7) 0.0072(6) 0.0043(7) C16 0.0469(10) 0.0268(11) 0.0246(8) -0.0019(7) 0.0040(8) -0.0061(9) C17 0.0295(8) 0.0287(10) 0.0249(8) 0.0015(7) 0.0075(7) 0.0101(7) Mo 0.02201(8) 0.01616(8) 0.01745(7) 0.00090(5) 0.00439(5) 0.00244(5) O1 0.0196(5) 0.0239(7) 0.0151(5) 0.0006(4) -0.0012(4) -0.0003(4) O2 0.0674(9) 0.0361(9) 0.0368(7) 0.0079(6) 0.0221(7) 0.0269(7) O3 0.0261(6) 0.0450(10) 0.0757(10) -0.0102(8) 0.0097(6) -0.0067(6) O4 0.0421(7) 0.0518(10) 0.0228(6) 0.0091(6) 0.0063(5) 0.0125(6) O5 0.0730(10) 0.0515(11) 0.0487(8) -0.0005(8) -0.0046(7) -0.0371(9) O6 0.0501(8) 0.0536(10) 0.0293(6) 0.0121(6) 0.0074(6) 0.0253(7) P 0.01578(17) 0.0157(2) 0.01474(17) 0.00067(15) 0.00100(14) -0.00031(15) Si1 0.01662(19) 0.0164(2) 0.0213(2) -0.00142(17) 0.00047(16) -0.00056(16) Si2 0.01681(19) 0.0246(3) 0.01802(19) 0.00218(17) -0.00190(16) 0.00009(18) _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. ; 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 C1 O1 1.4803(16) . ? C1 C2 1.514(2) . ? C1 P 1.7940(13) . ? C1 H1A 1.0000 . ? C2 C3 1.517(2) . ? C2 C5 1.534(2) . ? C2 C4 1.544(2) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4C 0.9800 . ? C4 H4B 0.9800 . ? C4 H4A 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 P 1.8114(15) . ? C6 Si1 1.9116(15) . ? C6 Si2 1.9128(14) . ? C6 H6A 1.0000 . ? C7 Si1 1.8683(15) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 Si1 1.8680(17) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 Si1 1.8676(14) . ? C9 H9C 0.9800 . ? C9 H9B 0.9800 . ? C9 H9A 0.9800 . ? C10 Si2 1.8678(16) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si2 1.8704(16) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Si2 1.8646(18) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 O2 1.141(2) . ? C13 Mo 2.0158(17) . ? C14 O3 1.139(2) . ? C14 Mo 2.0403(18) . ? C15 O4 1.1357(19) . ? C15 Mo 2.0472(16) . ? C16 O5 1.137(2) . ? C16 Mo 2.0497(19) . ? C17 O6 1.1354(19) . ? C17 Mo 2.0517(17) . ? Mo P 2.4878(4) . ? O1 P 1.6767(10) . ? 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 O1 C1 C2 116.83(12) . . ? O1 C1 P 60.71(6) . . ? C2 C1 P 132.84(12) . . ? O1 C1 H1A 111.7 . . ? C2 C1 H1A 111.7 . . ? P C1 H1A 111.7 . . ? C1 C2 C3 113.85(12) . . ? C1 C2 C5 107.25(13) . . ? C3 C2 C5 110.66(15) . . ? C1 C2 C4 106.03(14) . . ? C3 C2 C4 109.55(14) . . ? C5 C2 C4 109.32(12) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4C 109.5 . . ? C2 C4 H4B 109.5 . . ? H4C C4 H4B 109.5 . . ? C2 C4 H4A 109.5 . . ? H4C C4 H4A 109.5 . . ? H4B C4 H4A 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P C6 Si1 114.22(7) . . ? P C6 Si2 112.82(8) . . ? Si1 C6 Si2 117.60(8) . . ? P C6 H6A 103.3 . . ? Si1 C6 H6A 103.3 . . ? Si2 C6 H6A 103.3 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C9 H9C 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9C C9 H9B 109.5 . . ? Si1 C9 H9A 109.5 . . ? H9C C9 H9A 109.5 . . ? H9B C9 H9A 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C13 Mo 178.82(17) . . ? O3 C14 Mo 178.17(15) . . ? O4 C15 Mo 178.29(14) . . ? O5 C16 Mo 178.95(18) . . ? O6 C17 Mo 177.67(14) . . ? C13 Mo C14 88.15(7) . . ? C13 Mo C15 88.98(6) . . ? C14 Mo C15 89.85(7) . . ? C13 Mo C16 90.84(7) . . ? C14 Mo C16 178.71(7) . . ? C15 Mo C16 90.93(7) . . ? C13 Mo C17 89.14(6) . . ? C14 Mo C17 88.75(7) . . ? C15 Mo C17 177.69(6) . . ? C16 Mo C17 90.44(7) . . ? C13 Mo P 175.92(5) . . ? C14 Mo P 87.89(5) . . ? C15 Mo P 90.04(4) . . ? C16 Mo P 93.14(5) . . ? C17 Mo P 91.75(4) . . ? C1 O1 P 68.94(7) . . ? O1 P C1 50.35(5) . . ? O1 P C6 106.84(6) . . ? C1 P C6 104.43(7) . . ? O1 P Mo 120.23(4) . . ? C1 P Mo 136.75(6) . . ? C6 P Mo 117.49(4) . . ? C9 Si1 C8 106.69(7) . . ? C9 Si1 C7 110.87(7) . . ? C8 Si1 C7 108.67(8) . . ? C9 Si1 C6 114.89(7) . . ? C8 Si1 C6 108.23(7) . . ? C7 Si1 C6 107.34(7) . . ? C12 Si2 C10 107.80(8) . . ? C12 Si2 C11 108.31(8) . . ? C10 Si2 C11 109.88(9) . . ? C12 Si2 C6 110.64(7) . . ? C10 Si2 C6 107.88(7) . . ? C11 Si2 C6 112.25(7) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.482 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.075 #------------------------------------------------------------------------------ data_Greg1088f _database_code_depnum_ccdc_archive 'CCDC 792194' #TrackingRef 'Gesamtcif.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H21 Mo O6 P' _chemical_formula_sum 'C22 H21 Mo O6 P' _chemical_formula_weight 508.30 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4496(3) _cell_length_b 10.3509(3) _cell_length_c 13.0818(4) _cell_angle_alpha 101.544(2) _cell_angle_beta 109.683(2) _cell_angle_gamma 102.938(2) _cell_volume 1120.03(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9897 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 32.46 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 0.691 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.7693 _exptl_absorpt_correction_T_max 0.9467 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8-KappaApexII' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16877 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5394 _reflns_number_gt 4831 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+0.5944P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5394 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0618 _refine_ls_wR_factor_gt 0.0592 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.24996(19) 0.89489(18) 0.87808(15) 0.0191(3) Uani 1 1 d . . . H1A H 0.3033 0.9769 0.8600 0.023 Uiso 1 1 calc R . . C2 C 0.35569(19) 0.82010(17) 0.93352(15) 0.0200(4) Uani 1 1 d . . . C3 C 0.4764(2) 0.8054(2) 0.89909(17) 0.0273(4) Uani 1 1 d . . . H3A H 0.4899 0.8427 0.8410 0.033 Uiso 1 1 calc R . . C4 C 0.5775(2) 0.7364(2) 0.94922(19) 0.0325(5) Uani 1 1 d . . . H4A H 0.6601 0.7267 0.9254 0.039 Uiso 1 1 calc R . . C5 C 0.5588(2) 0.6818(2) 1.03337(18) 0.0302(5) Uani 1 1 d . . . H5A H 0.6274 0.6335 1.0667 0.036 Uiso 1 1 calc R . . C6 C 0.4400(2) 0.6974(2) 1.06942(17) 0.0284(4) Uani 1 1 d . . . H6A H 0.4282 0.6609 1.1282 0.034 Uiso 1 1 calc R . . C7 C 0.3378(2) 0.76660(19) 1.01957(15) 0.0229(4) Uani 1 1 d . . . H7A H 0.2562 0.7772 1.0442 0.027 Uiso 1 1 calc R . . C8 C -0.0250(2) 0.92609(17) 0.70278(14) 0.0172(3) Uani 1 1 d . . . C9 C -0.1838(2) 0.92572(17) 0.70626(15) 0.0182(3) Uani 1 1 d . . . C10 C -0.2973(2) 0.86267(17) 0.60022(15) 0.0196(4) Uani 1 1 d . . . C11 C -0.2249(2) 0.81534(17) 0.52238(14) 0.0194(4) Uani 1 1 d . . . C12 C -0.0667(2) 0.85083(17) 0.57984(14) 0.0184(3) Uani 1 1 d . . . C13 C 0.0918(2) 1.07339(18) 0.74517(16) 0.0247(4) Uani 1 1 d . . . H13A H 0.1245 1.1110 0.8275 0.037 Uiso 1 1 calc R . . H13B H 0.0405 1.1328 0.7065 0.037 Uiso 1 1 calc R . . H13C H 0.1850 1.0707 0.7287 0.037 Uiso 1 1 calc R . . C14 C -0.1991(2) 0.9905(2) 0.81312(16) 0.0257(4) Uani 1 1 d . . . H14A H -0.1215 1.0837 0.8505 0.039 Uiso 1 1 calc R . . H14B H -0.1797 0.9331 0.8643 0.039 Uiso 1 1 calc R . . H14C H -0.3062 0.9973 0.7947 0.039 Uiso 1 1 calc R . . C15 C -0.4719(2) 0.8421(2) 0.56207(18) 0.0302(4) Uani 1 1 d . . . H15A H -0.4934 0.8859 0.6265 0.045 Uiso 1 1 calc R . . H15B H -0.5304 0.7425 0.5337 0.045 Uiso 1 1 calc R . . H15C H -0.5057 0.8845 0.5012 0.045 Uiso 1 1 calc R . . C16 C -0.3215(2) 0.7417(2) 0.39811(16) 0.0283(4) Uani 1 1 d . . . H16A H -0.3730 0.8030 0.3625 0.043 Uiso 1 1 calc R . . H16B H -0.4024 0.6573 0.3891 0.043 Uiso 1 1 calc R . . H16C H -0.2523 0.7167 0.3616 0.043 Uiso 1 1 calc R . . C17 C 0.0567(2) 0.8274(2) 0.53700(16) 0.0257(4) Uani 1 1 d . . . H17A H 0.1281 0.7909 0.5884 0.038 Uiso 1 1 calc R . . H17B H 0.1176 0.9156 0.5339 0.038 Uiso 1 1 calc R . . H17C H 0.0052 0.7604 0.4606 0.038 Uiso 1 1 calc R . . C18 C -0.2126(2) 0.36337(19) 0.72584(16) 0.0238(4) Uani 1 1 d . . . C19 C -0.3208(2) 0.59815(18) 0.70526(16) 0.0236(4) Uani 1 1 d . . . C20 C -0.1482(2) 0.51794(18) 0.57471(16) 0.0223(4) Uani 1 1 d . . . C21 C 0.0998(2) 0.51100(18) 0.77708(15) 0.0217(4) Uani 1 1 d . . . C22 C -0.0745(2) 0.60900(18) 0.91308(16) 0.0214(4) Uani 1 1 d . . . O1 O 0.12992(14) 0.91383(12) 0.92195(10) 0.0198(3) Uani 1 1 d . . . O2 O -0.26864(17) 0.25066(14) 0.71917(13) 0.0348(4) Uani 1 1 d . . . O3 O -0.44432(16) 0.60868(15) 0.68253(14) 0.0354(4) Uani 1 1 d . . . O4 O -0.17662(16) 0.48743(14) 0.47980(11) 0.0288(3) Uani 1 1 d . . . O5 O 0.20488(16) 0.47132(15) 0.78915(12) 0.0320(3) Uani 1 1 d . . . O6 O -0.06192(17) 0.63342(15) 1.00525(12) 0.0297(3) Uani 1 1 d . . . P P 0.04263(5) 0.81102(4) 0.78738(4) 0.01549(9) Uani 1 1 d . . . Mo Mo -0.106084(16) 0.563705(14) 0.745360(12) 0.01639(5) Uani 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 C1 0.0188(8) 0.0179(8) 0.0170(8) 0.0048(7) 0.0045(7) 0.0036(6) C2 0.0166(8) 0.0161(8) 0.0182(9) 0.0007(7) 0.0005(7) 0.0024(6) C3 0.0212(9) 0.0275(10) 0.0285(10) 0.0059(8) 0.0075(8) 0.0049(7) C4 0.0213(9) 0.0303(11) 0.0400(12) 0.0040(9) 0.0083(8) 0.0093(8) C5 0.0220(9) 0.0213(9) 0.0329(11) 0.0026(8) -0.0038(8) 0.0077(7) C6 0.0308(10) 0.0227(9) 0.0209(10) 0.0050(7) -0.0002(8) 0.0065(8) C7 0.0213(8) 0.0226(9) 0.0188(9) 0.0040(7) 0.0022(7) 0.0067(7) C8 0.0214(8) 0.0133(8) 0.0137(8) 0.0058(6) 0.0037(6) 0.0032(6) C9 0.0249(9) 0.0129(8) 0.0186(8) 0.0074(6) 0.0087(7) 0.0071(6) C10 0.0228(8) 0.0161(8) 0.0198(9) 0.0099(7) 0.0063(7) 0.0057(6) C11 0.0264(9) 0.0131(8) 0.0148(8) 0.0065(6) 0.0042(7) 0.0029(6) C12 0.0265(9) 0.0145(8) 0.0151(8) 0.0072(6) 0.0083(7) 0.0060(6) C13 0.0273(9) 0.0163(8) 0.0229(9) 0.0080(7) 0.0037(8) 0.0007(7) C14 0.0349(10) 0.0247(9) 0.0212(9) 0.0080(7) 0.0123(8) 0.0136(8) C15 0.0238(9) 0.0350(11) 0.0308(11) 0.0166(9) 0.0058(8) 0.0093(8) C16 0.0336(10) 0.0248(10) 0.0156(9) 0.0042(7) 0.0035(8) 0.0004(8) C17 0.0313(10) 0.0280(10) 0.0233(10) 0.0119(8) 0.0146(8) 0.0101(8) C18 0.0245(9) 0.0217(9) 0.0200(9) 0.0087(7) 0.0016(7) 0.0067(7) C19 0.0231(9) 0.0167(8) 0.0266(10) 0.0094(7) 0.0054(7) 0.0023(7) C20 0.0208(8) 0.0158(8) 0.0254(10) 0.0074(7) 0.0042(7) 0.0035(6) C21 0.0261(9) 0.0179(8) 0.0160(9) 0.0034(7) 0.0041(7) 0.0059(7) C22 0.0215(8) 0.0174(8) 0.0257(10) 0.0094(7) 0.0072(7) 0.0078(7) O1 0.0219(6) 0.0203(6) 0.0141(6) 0.0031(5) 0.0041(5) 0.0076(5) O2 0.0372(8) 0.0200(7) 0.0352(8) 0.0137(6) 0.0017(6) 0.0015(6) O3 0.0216(7) 0.0298(8) 0.0553(10) 0.0227(7) 0.0105(7) 0.0081(6) O4 0.0346(7) 0.0285(7) 0.0184(7) 0.0051(6) 0.0068(6) 0.0088(6) O5 0.0310(7) 0.0320(8) 0.0283(8) 0.0034(6) 0.0048(6) 0.0176(6) O6 0.0375(8) 0.0338(8) 0.0223(7) 0.0112(6) 0.0136(6) 0.0145(6) P 0.0171(2) 0.0142(2) 0.0128(2) 0.00473(16) 0.00357(16) 0.00353(15) Mo 0.01816(8) 0.01310(8) 0.01503(8) 0.00607(5) 0.00292(6) 0.00374(5) _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. ; 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 C1 O1 1.465(2) . ? C1 C2 1.485(2) . ? C1 P 1.8056(17) . ? C1 H1A 1.0000 . ? C2 C3 1.387(3) . ? C2 C7 1.392(3) . ? C3 C4 1.387(3) . ? C3 H3A 0.9500 . ? C4 C5 1.378(3) . ? C4 H4A 0.9500 . ? C5 C6 1.384(3) . ? C5 H5A 0.9500 . ? C6 C7 1.394(3) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C12 1.511(2) . ? C8 C9 1.516(2) . ? C8 C13 1.532(2) . ? C8 P 1.8557(17) . ? C9 C10 1.350(2) . ? C9 C14 1.493(3) . ? C10 C11 1.471(3) . ? C10 C15 1.504(3) . ? C11 C12 1.350(2) . ? C11 C16 1.500(2) . ? C12 C17 1.498(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O2 1.141(2) . ? C18 Mo 2.0145(18) . ? C19 O3 1.140(2) . ? C19 Mo 2.0494(19) . ? C20 O4 1.138(2) . ? C20 Mo 2.064(2) . ? C21 O5 1.132(2) . ? C21 Mo 2.0682(19) . ? C22 O6 1.140(2) . ? C22 Mo 2.051(2) . ? O1 P 1.6706(12) . ? P Mo 2.4770(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 O1 C1 C2 116.31(15) . . ? O1 C1 P 60.36(8) . . ? C2 C1 P 123.27(12) . . ? O1 C1 H1A 115.2 . . ? C2 C1 H1A 115.2 . . ? P C1 H1A 115.2 . . ? C3 C2 C7 119.58(17) . . ? C3 C2 C1 118.65(17) . . ? C7 C2 C1 121.76(17) . . ? C4 C3 C2 120.2(2) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C5 C4 C3 120.3(2) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? C4 C5 C6 120.01(18) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C5 C6 C7 120.08(19) . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C2 C7 C6 119.81(19) . . ? C2 C7 H7A 120.1 . . ? C6 C7 H7A 120.1 . . ? C12 C8 C9 103.69(13) . . ? C12 C8 C13 113.94(15) . . ? C9 C8 C13 112.09(15) . . ? C12 C8 P 106.90(11) . . ? C9 C8 P 105.30(11) . . ? C13 C8 P 114.03(11) . . ? C10 C9 C14 129.28(17) . . ? C10 C9 C8 108.47(16) . . ? C14 C9 C8 122.22(15) . . ? C9 C10 C11 109.55(16) . . ? C9 C10 C15 127.38(18) . . ? C11 C10 C15 123.07(16) . . ? C12 C11 C10 109.81(15) . . ? C12 C11 C16 128.21(18) . . ? C10 C11 C16 121.97(16) . . ? C11 C12 C17 129.38(17) . . ? C11 C12 C8 108.46(15) . . ? C17 C12 C8 122.15(15) . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O2 C18 Mo 177.20(16) . . ? O3 C19 Mo 175.61(15) . . ? O4 C20 Mo 176.94(15) . . ? O5 C21 Mo 174.35(15) . . ? O6 C22 Mo 177.89(15) . . ? C1 O1 P 69.96(8) . . ? O1 P C1 49.68(7) . . ? O1 P C8 104.44(7) . . ? C1 P C8 107.98(8) . . ? O1 P Mo 119.51(5) . . ? C1 P Mo 125.61(6) . . ? C8 P Mo 124.63(5) . . ? C18 Mo C19 89.68(7) . . ? C18 Mo C22 88.40(7) . . ? C19 Mo C22 89.38(7) . . ? C18 Mo C20 91.10(7) . . ? C19 Mo C20 88.09(7) . . ? C22 Mo C20 177.43(7) . . ? C18 Mo C21 85.87(7) . . ? C19 Mo C21 174.96(7) . . ? C22 Mo C21 92.87(7) . . ? C20 Mo C21 89.61(7) . . ? C18 Mo P 174.55(5) . . ? C19 Mo P 93.64(5) . . ? C22 Mo P 87.32(5) . . ? C20 Mo P 93.32(5) . . ? C21 Mo P 90.97(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.589 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.067 #------------------------------------------------------------------------------ data_Greg998f _database_code_depnum_ccdc_archive 'CCDC 792195' #TrackingRef 'Gesamtcif.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H25 Mo O6 P' _chemical_formula_sum 'C20 H25 Mo O6 P' _chemical_formula_weight 488.31 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7742(4) _cell_length_b 10.7422(4) _cell_length_c 11.7769(5) _cell_angle_alpha 85.712(2) _cell_angle_beta 84.477(2) _cell_angle_gamma 89.652(2) _cell_volume 1101.78(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9418 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 37.38 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 0.699 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.6791 _exptl_absorpt_correction_T_max 0.8934 _exptl_absorpt_process_details 'Sadabs 2009/2' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2.00 1.00 0.00 0.1740 -2.00 -1.00 0.00 0.2120 1.00 -1.00 2.00 0.3110 -1.00 1.00 -2.00 0.4950 1.00 -1.00 -2.00 0.0770 -1.00 1.00 2.00 0.0050 _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8-KappaApexII' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41629 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5318 _reflns_number_gt 5158 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+1.0842P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5318 _refine_ls_number_parameters 272 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0580 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6404(2) 0.61482(15) 0.75437(14) 0.0253(3) Uani 1 1 d . . . C2 C 0.6976(2) 0.61964(15) 0.62865(16) 0.0278(4) Uani 1 1 d . . . C3 C 0.5812(2) 0.65692(16) 0.56720(14) 0.0298(4) Uani 1 1 d . . . C4 C 0.4449(2) 0.68035(17) 0.64431(16) 0.0307(4) Uani 1 1 d . . . C5 C 0.4775(2) 0.65953(18) 0.75290(15) 0.0285(4) Uani 1 1 d . . . C6 C 0.6494(3) 0.48155(18) 0.81052(19) 0.0450(6) Uani 1 1 d . . . H6A H 0.7565 0.4601 0.8193 0.068 Uiso 1 1 calc R . . H6B H 0.6066 0.4228 0.7622 0.068 Uiso 1 1 calc R . . H6C H 0.5907 0.4767 0.8859 0.068 Uiso 1 1 calc R . . C7 C 0.8551(3) 0.5793(2) 0.5877(2) 0.0487(6) Uani 1 1 d . . . H7A H 0.8648 0.4890 0.6042 0.073 Uiso 1 1 calc R . . H7B H 0.9302 0.6227 0.6269 0.073 Uiso 1 1 calc R . . H7C H 0.8736 0.5997 0.5050 0.073 Uiso 1 1 calc R . . C8 C 0.5810(4) 0.6711(2) 0.43942(17) 0.0514(7) Uani 1 1 d . . . H8A H 0.5096 0.6107 0.4153 0.077 Uiso 1 1 calc R . . H8B H 0.6843 0.6559 0.4036 0.077 Uiso 1 1 calc R . . H8C H 0.5489 0.7559 0.4159 0.077 Uiso 1 1 calc R . . C9 C 0.2929(3) 0.7185(3) 0.6032(2) 0.0549(7) Uani 1 1 d . . . H9A H 0.2623 0.6585 0.5509 0.082 Uiso 1 1 calc R . . H9B H 0.3019 0.8018 0.5631 0.082 Uiso 1 1 calc R . . H9C H 0.2155 0.7201 0.6689 0.082 Uiso 1 1 calc R . . C10 C 0.3746(3) 0.6746(3) 0.8606(2) 0.0537(7) Uani 1 1 d . . . H10A H 0.4080 0.7469 0.8979 0.081 Uiso 1 1 calc R . . H10B H 0.3797 0.5993 0.9124 0.081 Uiso 1 1 calc R . . H10C H 0.2690 0.6875 0.8416 0.081 Uiso 1 1 calc R . . C11 C 0.7877(3) 0.66542(17) 0.95788(17) 0.0357(5) Uani 1 1 d . A . H11A H 0.7313 0.5849 0.9779 0.043 Uiso 1 1 calc R . . C12 C 0.8373(3) 0.72184(16) 1.06328(18) 0.0391(5) Uani 1 1 d D . . C13 C 0.6924(3) 0.7745(3) 1.12782(18) 0.0552(7) Uani 1 1 d . A . H13C H 0.7195 0.8086 1.1981 0.083 Uiso 1 1 calc R . . H13B H 0.6170 0.7076 1.1472 0.083 Uiso 1 1 calc R . . H13A H 0.6489 0.8408 1.0791 0.083 Uiso 1 1 calc R . . C14 C 0.9329(7) 0.6168(3) 1.1200(6) 0.0366(14) Uani 0.520(13) 1 d PDU A 1 H14A H 1.0223 0.5982 1.0675 0.055 Uiso 0.520(13) 1 calc PR A 1 H14B H 0.8697 0.5416 1.1373 0.055 Uiso 0.520(13) 1 calc PR A 1 H14C H 0.9669 0.6442 1.1909 0.055 Uiso 0.520(13) 1 calc PR A 1 C14S C 0.8678(7) 0.6180(3) 1.1556(4) 0.0267(13) Uani 0.480(13) 1 d PDU A 2 H14D H 0.9523 0.5654 1.1265 0.040 Uiso 0.480(13) 1 calc PR A 2 H14E H 0.7755 0.5670 1.1748 0.040 Uiso 0.480(13) 1 calc PR A 2 H14F H 0.8952 0.6556 1.2242 0.040 Uiso 0.480(13) 1 calc PR A 2 C15 C 0.9564(2) 0.82455(17) 1.03505(18) 0.0312(4) Uani 1 1 d . A . H15C H 0.9901 0.8521 1.1061 0.047 Uiso 1 1 calc R . . H15B H 0.9115 0.8952 0.9925 0.047 Uiso 1 1 calc R . . H15A H 1.0444 0.7926 0.9883 0.047 Uiso 1 1 calc R . . C16 C 0.8140(2) 1.13300(16) 0.67793(15) 0.0272(3) Uani 1 1 d U A . C17 C 0.7017(2) 1.02366(17) 0.88676(15) 0.0268(3) Uani 1 1 d U A . C18 C 1.00062(19) 0.94302(16) 0.76431(16) 0.0272(3) Uani 1 1 d U A . C19 C 0.8349(2) 0.90195(16) 0.57069(16) 0.0282(4) Uani 1 1 d U A . C20 C 0.5540(2) 0.96980(17) 0.68754(15) 0.0265(3) Uani 1 1 d U A . O1 O 0.90523(18) 0.65684(12) 0.85905(14) 0.0394(4) Uani 1 1 d . . . O2 O 0.8405(2) 1.23579(13) 0.65252(13) 0.0442(4) Uani 1 1 d . . . O3 O 0.65904(18) 1.07000(17) 0.96754(13) 0.0447(4) Uani 1 1 d . . . O4 O 1.12690(16) 0.93866(17) 0.77746(15) 0.0469(4) Uani 1 1 d . . . O5 O 0.8666(2) 0.88191(14) 0.47798(13) 0.0448(4) Uani 1 1 d . . . O6 O 0.43724(16) 0.98700(15) 0.65533(14) 0.0414(3) Uani 1 1 d . . . P P 0.75022(5) 0.73445(4) 0.81952(4) 0.02369(9) Uani 1 1 d . A . Mo Mo 0.774301(14) 0.953996(11) 0.733661(11) 0.01744(5) Uani 1 1 d 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 C1 0.0361(9) 0.0193(7) 0.0214(8) 0.0048(6) -0.0122(7) -0.0137(7) C2 0.0392(10) 0.0148(7) 0.0285(9) -0.0030(6) 0.0022(7) -0.0084(7) C3 0.0557(12) 0.0169(7) 0.0172(7) 0.0002(6) -0.0063(7) -0.0101(7) C4 0.0394(10) 0.0276(9) 0.0278(9) -0.0047(7) -0.0145(8) -0.0075(7) C5 0.0312(9) 0.0325(9) 0.0225(8) -0.0027(7) -0.0043(7) -0.0170(7) C6 0.0783(16) 0.0217(9) 0.0394(11) 0.0118(8) -0.0364(11) -0.0257(10) C7 0.0444(12) 0.0260(10) 0.0751(17) -0.0175(10) 0.0089(11) -0.0036(9) C8 0.106(2) 0.0309(10) 0.0180(9) 0.0001(8) -0.0085(11) -0.0160(12) C9 0.0540(14) 0.0561(15) 0.0636(16) -0.0223(12) -0.0380(13) 0.0041(12) C10 0.0507(13) 0.0754(17) 0.0347(11) -0.0183(11) 0.0106(10) -0.0392(13) C11 0.0535(12) 0.0206(8) 0.0362(10) 0.0077(7) -0.0281(9) -0.0145(8) C12 0.0604(13) 0.0240(9) 0.0368(10) 0.0086(8) -0.0318(10) -0.0174(9) C13 0.0537(14) 0.0859(19) 0.0252(10) 0.0108(11) -0.0082(9) -0.0438(14) C14 0.045(2) 0.0318(17) 0.0351(19) 0.0027(13) -0.0189(16) -0.0052(14) C14S 0.033(2) 0.0249(16) 0.0232(17) -0.0004(12) -0.0091(14) -0.0010(13) C15 0.0270(9) 0.0267(9) 0.0431(10) -0.0104(8) -0.0140(8) -0.0023(7) C16 0.0399(10) 0.0175(6) 0.0248(8) -0.0009(6) -0.0060(7) -0.0024(7) C17 0.0225(8) 0.0315(9) 0.0264(7) -0.0026(6) -0.0022(6) 0.0063(7) C18 0.0211(7) 0.0227(8) 0.0375(9) -0.0083(7) 0.0033(6) -0.0018(6) C19 0.0325(9) 0.0200(8) 0.0305(8) -0.0045(6) 0.0087(7) -0.0084(7) C20 0.0237(7) 0.0258(8) 0.0295(9) 0.0003(7) -0.0013(6) 0.0018(6) O1 0.0495(9) 0.0197(6) 0.0546(9) -0.0062(6) -0.0318(7) 0.0039(6) O2 0.0761(11) 0.0176(6) 0.0412(8) 0.0039(6) -0.0207(8) -0.0087(7) O3 0.0367(8) 0.0677(11) 0.0314(7) -0.0177(7) -0.0017(6) 0.0180(7) O4 0.0197(7) 0.0578(10) 0.0639(11) -0.0175(8) 0.0021(6) -0.0007(6) O5 0.0603(10) 0.0366(8) 0.0341(8) -0.0103(6) 0.0199(7) -0.0166(7) O6 0.0278(7) 0.0435(8) 0.0532(9) 0.0028(7) -0.0107(6) 0.0053(6) P 0.0293(2) 0.01519(18) 0.0281(2) 0.00333(15) -0.01376(17) -0.00746(15) Mo 0.01777(7) 0.01232(7) 0.02152(7) -0.00076(5) 0.00149(5) -0.00109(5) _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. ; 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 C1 C5 1.507(3) . ? C1 C2 1.514(2) . ? C1 C6 1.536(2) . ? C1 P 1.8637(16) . ? C2 C3 1.350(3) . ? C2 C7 1.491(3) . ? C3 C4 1.463(3) . ? C3 C8 1.501(2) . ? C4 C5 1.339(2) . ? C4 C9 1.507(3) . ? C5 C10 1.502(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 O1 1.487(3) . ? C11 C12 1.522(3) . ? C11 P 1.7980(18) . ? C11 H11A 1.0000 . ? C12 C15 1.521(3) . ? C12 C14S 1.5386(19) . ? C12 C13 1.544(4) . ? C12 C14 1.5510(19) . ? C13 H13C 0.9800 . ? C13 H13B 0.9800 . ? C13 H13A 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14S H14D 0.9800 . ? C14S H14E 0.9800 . ? C14S H14F 0.9800 . ? C15 H15C 0.9800 . ? C15 H15B 0.9800 . ? C15 H15A 0.9800 . ? C16 O2 1.142(2) . ? C16 Mo 2.0063(17) . ? C17 O3 1.137(2) . ? C17 Mo 2.0472(18) . ? C18 O4 1.134(2) . ? C18 Mo 2.0534(18) . ? C19 O5 1.136(2) . ? C19 Mo 2.0590(18) . ? C20 O6 1.136(2) . ? C20 Mo 2.0599(18) . ? O1 P 1.6768(14) . ? P Mo 2.4975(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 C5 C1 C2 103.10(14) . . ? C5 C1 C6 111.92(16) . . ? C2 C1 C6 111.07(16) . . ? C5 C1 P 107.90(12) . . ? C2 C1 P 106.91(11) . . ? C6 C1 P 115.13(12) . . ? C3 C2 C7 129.09(19) . . ? C3 C2 C1 108.36(16) . . ? C7 C2 C1 122.42(19) . . ? C2 C3 C4 109.79(15) . . ? C2 C3 C8 127.9(2) . . ? C4 C3 C8 122.2(2) . . ? C5 C4 C3 109.44(17) . . ? C5 C4 C9 127.2(2) . . ? C3 C4 C9 123.36(18) . . ? C4 C5 C10 128.3(2) . . ? C4 C5 C1 109.25(17) . . ? C10 C5 C1 122.46(18) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 C12 117.22(17) . . ? O1 C11 P 60.51(9) . . ? C12 C11 P 131.91(13) . . ? O1 C11 H11A 112.0 . . ? C12 C11 H11A 112.0 . . ? P C11 H11A 112.0 . . ? C15 C12 C11 113.31(17) . . ? C15 C12 C14S 118.0(2) . . ? C11 C12 C14S 110.3(2) . . ? C15 C12 C13 109.81(17) . . ? C11 C12 C13 107.26(17) . . ? C14S C12 C13 96.4(3) . . ? C15 C12 C14 101.5(3) . . ? C11 C12 C14 103.8(2) . . ? C14S C12 C14 25.2(2) . . ? C13 C12 C14 121.2(3) . . ? C12 C13 H13C 109.5 . . ? C12 C13 H13B 109.5 . . ? H13C C13 H13B 109.5 . . ? C12 C13 H13A 109.5 . . ? H13C C13 H13A 109.5 . . ? H13B C13 H13A 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? C12 C14S H14D 109.5 . . ? C12 C14S H14E 109.5 . . ? H14D C14S H14E 109.5 . . ? C12 C14S H14F 109.5 . . ? H14D C14S H14F 109.5 . . ? H14E C14S H14F 109.5 . . ? C12 C15 H15C 109.5 . . ? C12 C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? C12 C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? O2 C16 Mo 175.69(16) . . ? O3 C17 Mo 175.15(17) . . ? O4 C18 Mo 177.62(18) . . ? O5 C19 Mo 175.05(17) . . ? O6 C20 Mo 173.89(16) . . ? C11 O1 P 68.97(10) . . ? O1 P C11 50.51(10) . . ? O1 P C1 103.75(8) . . ? C11 P C1 105.62(8) . . ? O1 P Mo 120.24(6) . . ? C11 P Mo 131.55(6) . . ? C1 P Mo 121.53(5) . . ? C16 Mo C17 85.10(7) . . ? C16 Mo C18 87.27(7) . . ? C17 Mo C18 94.99(7) . . ? C16 Mo C19 89.61(7) . . ? C17 Mo C19 173.21(7) . . ? C18 Mo C19 88.98(7) . . ? C16 Mo C20 89.94(7) . . ? C17 Mo C20 89.20(7) . . ? C18 Mo C20 174.75(7) . . ? C19 Mo C20 86.55(8) . . ? C16 Mo P 172.81(5) . . ? C17 Mo P 91.78(5) . . ? C18 Mo P 86.55(5) . . ? C19 Mo P 93.95(5) . . ? C20 Mo P 96.50(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.596 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.066 #------------------------------------------------------------------------------ data_Greg1230b _database_code_depnum_ccdc_archive 'CCDC 792196' #TrackingRef 'Gesamtcif.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H22 Cl Cr O6 P' _chemical_formula_sum 'C22 H22 Cl Cr O6 P' _chemical_formula_weight 500.82 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.0457(9) _cell_length_b 9.8476(4) _cell_length_c 14.5174(9) _cell_angle_alpha 90.00 _cell_angle_beta 109.103(3) _cell_angle_gamma 90.00 _cell_volume 2302.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4557 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 29.13 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.6728 _exptl_absorpt_correction_T_max 0.8029 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14725 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_sigmaI/netI 0.0922 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5411 _reflns_number_gt 3603 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5411 _refine_ls_number_parameters 285 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0883 _refine_ls_wR_factor_gt 0.0790 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr Cr 0.39858(2) -0.64620(3) 0.15616(3) 0.01921(11) Uani 1 1 d U . . Cl Cl 0.18817(3) -0.52291(5) 0.06393(4) 0.02170(13) Uani 1 1 d . . . P P 0.26179(3) -0.66937(5) 0.15332(4) 0.01723(14) Uani 1 1 d . . . O1 O 0.15239(9) -0.67945(14) 0.24487(11) 0.0224(4) Uani 1 1 d . . . O2 O 0.57168(10) -0.56940(17) 0.16211(14) 0.0417(5) Uani 1 1 d . . . O3 O 0.38199(10) -0.34476(15) 0.19553(13) 0.0346(4) Uani 1 1 d U . . O4 O 0.46565(10) -0.72542(16) 0.37041(12) 0.0310(4) Uani 1 1 d . . . O5 O 0.44475(10) -0.93390(15) 0.11857(12) 0.0335(4) Uani 1 1 d U . . O6 O 0.33063(10) -0.60546(15) -0.06316(12) 0.0315(4) Uani 1 1 d . . . C1 C 0.23695(13) -0.6444(2) 0.26773(16) 0.0191(5) Uani 1 1 d . . . H1 H 0.2703 -0.7115 0.3167 0.023 Uiso 1 1 calc R . . C2 C 0.12799(13) -0.7967(2) 0.17849(16) 0.0194(5) Uani 1 1 d . . . C3 C 0.19357(13) -0.8235(2) 0.12544(16) 0.0197(5) Uani 1 1 d . . . C4 C 0.25277(13) -0.5057(2) 0.31400(16) 0.0191(5) Uani 1 1 d . . . C5 C 0.32413(14) -0.4813(2) 0.39161(17) 0.0273(5) Uani 1 1 d . . . H5 H 0.3629 -0.5528 0.4158 0.033 Uiso 1 1 calc R . . C6 C 0.33995(16) -0.3548(2) 0.43443(19) 0.0361(6) Uani 1 1 d . . . H6 H 0.3893 -0.3394 0.4877 0.043 Uiso 1 1 calc R . . C7 C 0.28378(16) -0.2505(2) 0.3995(2) 0.0353(6) Uani 1 1 d . . . H7 H 0.2948 -0.1628 0.4282 0.042 Uiso 1 1 calc R . . C8 C 0.21181(15) -0.2738(2) 0.32317(18) 0.0312(6) Uani 1 1 d . . . H8 H 0.1729 -0.2023 0.2998 0.037 Uiso 1 1 calc R . . C9 C 0.19587(14) -0.4010(2) 0.28015(17) 0.0226(5) Uani 1 1 d . . . H9 H 0.1461 -0.4166 0.2276 0.027 Uiso 1 1 calc R . . C10 C 0.05140(13) -0.7557(2) 0.09702(17) 0.0220(5) Uani 1 1 d . . . C11 C 0.05929(13) -0.7730(2) 0.00993(17) 0.0234(5) Uani 1 1 d . . . C12 C 0.14172(14) -0.8368(2) 0.01588(16) 0.0226(5) Uani 1 1 d . . . H12 H 0.1684 -0.7819 -0.0238 0.027 Uiso 1 1 calc R . . C13 C 0.11415(14) -0.9141(2) 0.23978(17) 0.0260(5) Uani 1 1 d . . . H13A H 0.1657 -0.9327 0.2931 0.039 Uiso 1 1 calc R . . H13B H 0.0975 -0.9951 0.1989 0.039 Uiso 1 1 calc R . . H13C H 0.0703 -0.8899 0.2668 0.039 Uiso 1 1 calc R . . C14 C -0.02120(14) -0.6981(2) 0.12111(18) 0.0320(6) Uani 1 1 d . . . H14A H -0.0649 -0.6720 0.0608 0.048 Uiso 1 1 calc R . . H14B H -0.0033 -0.6181 0.1628 0.048 Uiso 1 1 calc R . . H14C H -0.0428 -0.7667 0.1554 0.048 Uiso 1 1 calc R . . C15 C -0.00307(15) -0.7366(3) -0.08673(17) 0.0353(6) Uani 1 1 d . . . H15A H -0.0588 -0.7356 -0.0810 0.053 Uiso 1 1 calc R . . H15B H -0.0010 -0.8040 -0.1356 0.053 Uiso 1 1 calc R . . H15C H 0.0099 -0.6466 -0.1067 0.053 Uiso 1 1 calc R . . C16 C 0.12856(15) -0.9823(2) -0.02325(19) 0.0331(6) Uani 1 1 d . . . H16A H 0.1005 -1.0353 0.0139 0.050 Uiso 1 1 calc R . . H16B H 0.1824 -1.0236 -0.0165 0.050 Uiso 1 1 calc R . . H16C H 0.0943 -0.9810 -0.0922 0.050 Uiso 1 1 calc R . . C17 C 0.25267(13) -0.9441(2) 0.16655(17) 0.0250(5) Uani 1 1 d . . . H17A H 0.2200 -1.0266 0.1646 0.037 Uiso 1 1 calc R . . H17B H 0.2865 -0.9248 0.2341 0.037 Uiso 1 1 calc R . . H17C H 0.2889 -0.9575 0.1270 0.037 Uiso 1 1 calc R . . C18 C 0.50673(14) -0.6005(2) 0.15989(18) 0.0265(5) Uani 1 1 d U . . C19 C 0.38606(13) -0.4582(2) 0.18132(17) 0.0231(5) Uani 1 1 d U . . C20 C 0.43906(13) -0.6917(2) 0.29044(17) 0.0221(5) Uani 1 1 d U . . C21 C 0.42334(13) -0.8273(2) 0.13212(16) 0.0231(5) Uani 1 1 d U . . C22 C 0.35652(14) -0.6187(2) 0.01994(18) 0.0215(5) Uani 1 1 d 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 Cr 0.0144(2) 0.01750(18) 0.0251(2) -0.00085(15) 0.00558(16) -0.00115(14) Cl 0.0172(3) 0.0202(3) 0.0255(3) 0.0043(2) 0.0041(2) 0.0025(2) P 0.0140(3) 0.0161(3) 0.0205(3) 0.0004(2) 0.0042(3) -0.0003(2) O1 0.0198(9) 0.0216(8) 0.0278(9) -0.0067(7) 0.0103(7) -0.0056(6) O2 0.0232(10) 0.0407(10) 0.0657(14) -0.0026(9) 0.0209(10) -0.0070(8) O3 0.0323(10) 0.0217(8) 0.0503(12) -0.0056(8) 0.0143(9) -0.0044(7) O4 0.0262(10) 0.0323(9) 0.0303(10) 0.0018(8) 0.0035(8) 0.0014(7) O5 0.0313(10) 0.0253(8) 0.0400(11) -0.0037(8) 0.0063(9) 0.0062(7) O6 0.0401(11) 0.0276(9) 0.0278(10) 0.0004(8) 0.0125(9) 0.0006(7) C1 0.0159(12) 0.0196(11) 0.0198(12) 0.0003(9) 0.0030(10) 0.0011(9) C2 0.0199(12) 0.0174(10) 0.0215(12) -0.0037(9) 0.0076(10) -0.0055(9) C3 0.0148(11) 0.0182(11) 0.0264(13) -0.0035(10) 0.0071(10) -0.0035(8) C4 0.0192(12) 0.0169(10) 0.0223(12) -0.0003(9) 0.0083(10) -0.0025(9) C5 0.0237(13) 0.0264(12) 0.0298(14) -0.0027(11) 0.0062(11) 0.0025(10) C6 0.0268(14) 0.0374(14) 0.0399(16) -0.0166(12) 0.0054(13) -0.0086(11) C7 0.0410(16) 0.0205(12) 0.0500(17) -0.0111(12) 0.0224(14) -0.0095(11) C8 0.0387(16) 0.0181(11) 0.0440(16) 0.0025(11) 0.0232(14) 0.0035(10) C9 0.0209(12) 0.0218(11) 0.0263(13) 0.0002(10) 0.0095(11) 0.0006(9) C10 0.0154(12) 0.0187(11) 0.0307(14) 0.0029(10) 0.0058(11) -0.0011(9) C11 0.0168(12) 0.0245(12) 0.0267(13) 0.0017(10) 0.0043(11) -0.0046(9) C12 0.0201(12) 0.0248(12) 0.0231(13) -0.0039(10) 0.0077(10) -0.0083(9) C13 0.0265(13) 0.0222(12) 0.0316(14) 0.0012(11) 0.0125(11) -0.0025(10) C14 0.0204(13) 0.0335(13) 0.0415(16) -0.0011(12) 0.0093(12) 0.0025(10) C15 0.0269(14) 0.0449(15) 0.0305(15) 0.0020(12) 0.0044(12) -0.0067(12) C16 0.0310(15) 0.0343(14) 0.0354(15) -0.0120(12) 0.0129(13) -0.0078(11) C17 0.0217(13) 0.0189(11) 0.0342(14) 0.0003(10) 0.0090(11) 0.0000(9) C18 0.0193(10) 0.0249(12) 0.0353(15) -0.0021(11) 0.0090(12) -0.0029(9) C19 0.0175(12) 0.0221(8) 0.0290(13) -0.0014(10) 0.0069(10) -0.0031(9) C20 0.0138(12) 0.0229(11) 0.0266(9) -0.0044(10) 0.0026(10) 0.0018(9) C21 0.0176(12) 0.0238(9) 0.0249(13) -0.0029(10) 0.0029(10) -0.0001(9) C22 0.0210(13) 0.0160(10) 0.0279(9) -0.0014(10) 0.0086(10) 0.0010(9) _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. ; 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 Cr C18 1.881(2) . ? Cr C22 1.890(2) . ? Cr C21 1.891(2) . ? Cr C20 1.897(2) . ? Cr C19 1.913(2) . ? Cr P 2.3296(7) . ? Cl P 2.0672(7) . ? P C1 1.860(2) . ? P C3 1.874(2) . ? O1 C1 1.412(2) . ? O1 C2 1.474(2) . ? O2 C18 1.139(3) . ? O3 C19 1.142(2) . ? O4 C20 1.148(3) . ? O5 C21 1.149(2) . ? O6 C22 1.148(3) . ? C1 C4 1.507(3) . ? C1 H1 1.0000 . ? C2 C10 1.502(3) . ? C2 C13 1.523(3) . ? C2 C3 1.573(3) . ? C3 C17 1.546(3) . ? C3 C12 1.552(3) . ? C4 C5 1.382(3) . ? C4 C9 1.391(3) . ? C5 C6 1.379(3) . ? C5 H5 0.9500 . ? C6 C7 1.382(3) . ? C6 H6 0.9500 . ? C7 C8 1.377(3) . ? C7 H7 0.9500 . ? C8 C9 1.386(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.325(3) . ? C10 C14 1.503(3) . ? C11 C15 1.500(3) . ? C11 C12 1.515(3) . ? C12 C16 1.531(3) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? 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 C18 Cr C22 91.63(10) . . ? C18 Cr C21 87.43(10) . . ? C22 Cr C21 88.47(9) . . ? C18 Cr C20 90.20(10) . . ? C22 Cr C20 174.56(9) . . ? C21 Cr C20 86.49(9) . . ? C18 Cr C19 86.12(9) . . ? C22 Cr C19 91.90(9) . . ? C21 Cr C19 173.54(9) . . ? C20 Cr C19 93.34(9) . . ? C18 Cr P 171.75(7) . . ? C22 Cr P 87.76(7) . . ? C21 Cr P 100.77(7) . . ? C20 Cr P 91.17(7) . . ? C19 Cr P 85.68(7) . . ? C1 P C3 89.62(9) . . ? C1 P Cl 101.51(7) . . ? C3 P Cl 102.89(7) . . ? C1 P Cr 119.37(7) . . ? C3 P Cr 129.04(7) . . ? Cl P Cr 109.95(3) . . ? C1 O1 C2 113.14(15) . . ? O1 C1 C4 110.25(17) . . ? O1 C1 P 105.73(14) . . ? C4 C1 P 117.26(15) . . ? O1 C1 H1 107.7 . . ? C4 C1 H1 107.7 . . ? P C1 H1 107.7 . . ? O1 C2 C10 106.92(17) . . ? O1 C2 C13 106.08(17) . . ? C10 C2 C13 113.76(18) . . ? O1 C2 C3 110.96(16) . . ? C10 C2 C3 103.49(17) . . ? C13 C2 C3 115.42(17) . . ? C17 C3 C12 114.31(17) . . ? C17 C3 C2 114.68(18) . . ? C12 C3 C2 104.96(17) . . ? C17 C3 P 105.02(14) . . ? C12 C3 P 113.24(14) . . ? C2 C3 P 104.39(13) . . ? C5 C4 C9 119.02(19) . . ? C5 C4 C1 120.15(19) . . ? C9 C4 C1 120.82(19) . . ? C6 C5 C4 121.0(2) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 119.8(2) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C6 119.9(2) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 120.3(2) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C8 C9 C4 120.0(2) . . ? C8 C9 H9 120.0 . . ? C4 C9 H9 120.0 . . ? C11 C10 C2 112.5(2) . . ? C11 C10 C14 128.2(2) . . ? C2 C10 C14 119.2(2) . . ? C10 C11 C15 126.8(2) . . ? C10 C11 C12 112.4(2) . . ? C15 C11 C12 120.8(2) . . ? C11 C12 C16 110.25(18) . . ? C11 C12 C3 103.30(18) . . ? C16 C12 C3 115.11(19) . . ? C11 C12 H12 109.3 . . ? C16 C12 H12 109.3 . . ? C3 C12 H12 109.3 . . ? C2 C13 H13A 109.5 . . ? C2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 H15A 109.5 . . ? C11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C3 C17 H17A 109.5 . . ? C3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O2 C18 Cr 178.2(2) . . ? O3 C19 Cr 176.8(2) . . ? O4 C20 Cr 176.21(19) . . ? O5 C21 Cr 174.5(2) . . ? O6 C22 Cr 178.24(19) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.496 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.080 #------------------------------------------------------------------------------ data_Greg1290 _database_code_depnum_ccdc_archive 'CCDC 792197' #TrackingRef 'Gesamtcif.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H22 Cl Mo O6 P' _chemical_formula_sum 'C22 H22 Cl Mo O6 P' _chemical_formula_weight 544.76 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' Cl Cl 0.1484 0.1585 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.3419(14) _cell_length_b 9.8710(9) _cell_length_c 14.7056(10) _cell_angle_alpha 90.00 _cell_angle_beta 109.209(5) _cell_angle_gamma 90.00 _cell_volume 2377.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5071 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 29.13 _exptl_crystal_description block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.766 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.7917 _exptl_absorpt_correction_T_max 0.7917 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15770 _diffrn_reflns_av_R_equivalents 0.0899 _diffrn_reflns_av_sigmaI/netI 0.1291 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5577 _reflns_number_gt 3098 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0010(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5577 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1124 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_restrained_S_all 0.912 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo 0.398150(19) -0.14657(4) 0.15635(2) 0.02806(13) Uani 1 1 d . . . Cl Cl 0.18364(5) -0.02298(10) 0.06397(6) 0.0289(2) Uani 1 1 d . . . P P 0.25549(6) -0.17068(11) 0.15274(7) 0.0273(3) Uani 1 1 d . . . O1 O 0.14792(14) -0.1804(3) 0.24279(17) 0.0335(7) Uani 1 1 d . . . O2 O 0.57574(18) -0.0672(3) 0.1625(2) 0.0539(9) Uani 1 1 d . . . O3 O 0.46826(16) -0.2296(3) 0.3782(2) 0.0431(8) Uani 1 1 d . . . O4 O 0.37787(17) 0.1682(3) 0.1963(2) 0.0491(8) Uani 1 1 d . . . O5 O 0.32578(17) -0.1021(3) -0.0702(2) 0.0427(8) Uani 1 1 d . . . O6 O 0.44236(18) -0.4469(3) 0.1143(2) 0.0498(8) Uani 1 1 d . . . C1 C 0.2313(2) -0.1451(4) 0.2659(3) 0.0293(9) Uani 1 1 d . . . H1A H 0.2641 -0.2120 0.3144 0.035 Uiso 1 1 calc R . . C2 C 0.1245(2) -0.2977(4) 0.1781(3) 0.0297(9) Uani 1 1 d . . . C3 C 0.1888(2) -0.3251(4) 0.1268(3) 0.0291(9) Uani 1 1 d . . . C4 C 0.2473(2) -0.0073(4) 0.3110(3) 0.0295(9) Uani 1 1 d . . . C5 C 0.3182(2) 0.0179(4) 0.3862(3) 0.0373(10) Uani 1 1 d . . . H5A H 0.3564 -0.0533 0.4098 0.045 Uiso 1 1 calc R . . C6 C 0.3346(3) 0.1439(5) 0.4273(3) 0.0466(12) Uani 1 1 d . . . H6A H 0.3840 0.1593 0.4786 0.056 Uiso 1 1 calc R . . C7 C 0.2802(3) 0.2475(5) 0.3949(3) 0.0495(12) Uani 1 1 d . . . H7A H 0.2918 0.3351 0.4228 0.059 Uiso 1 1 calc R . . C8 C 0.2075(3) 0.2230(4) 0.3205(3) 0.0417(11) Uani 1 1 d . . . H8A H 0.1687 0.2937 0.2984 0.050 Uiso 1 1 calc R . . C9 C 0.1918(2) 0.0970(4) 0.2791(3) 0.0323(10) Uani 1 1 d . . . H9A H 0.1422 0.0814 0.2280 0.039 Uiso 1 1 calc R . . C10 C 0.0489(2) -0.2580(4) 0.0968(3) 0.0330(10) Uani 1 1 d . . . C11 C 0.0574(2) -0.2759(4) 0.0111(3) 0.0370(11) Uani 1 1 d . . . C12 C 0.1385(2) -0.3388(4) 0.0174(3) 0.0368(10) Uani 1 1 d . . . H12A H 0.1649 -0.2829 -0.0209 0.044 Uiso 1 1 calc R . . C13 C 0.1102(2) -0.4131(4) 0.2379(3) 0.0364(10) Uani 1 1 d . . . H13A H 0.1604 -0.4311 0.2916 0.055 Uiso 1 1 calc R . . H13B H 0.0945 -0.4944 0.1978 0.055 Uiso 1 1 calc R . . H13C H 0.0664 -0.3887 0.2633 0.055 Uiso 1 1 calc R . . C14 C 0.2473(2) -0.4446(4) 0.1669(3) 0.0388(11) Uani 1 1 d . . . H14A H 0.2155 -0.5266 0.1670 0.058 Uiso 1 1 calc R . . H14B H 0.2821 -0.4240 0.2328 0.058 Uiso 1 1 calc R . . H14C H 0.2815 -0.4591 0.1264 0.058 Uiso 1 1 calc R . . C15 C -0.0226(2) -0.2000(5) 0.1197(3) 0.0478(12) Uani 1 1 d . . . H15A H -0.0055 -0.1180 0.1587 0.072 Uiso 1 1 calc R . . H15B H -0.0428 -0.2669 0.1556 0.072 Uiso 1 1 calc R . . H15C H -0.0661 -0.1773 0.0596 0.072 Uiso 1 1 calc R . . C16 C -0.0040(3) -0.2413(5) -0.0844(3) 0.0513(13) Uani 1 1 d . . . H16A H 0.0107 -0.1548 -0.1071 0.077 Uiso 1 1 calc R . . H16B H -0.0583 -0.2337 -0.0777 0.077 Uiso 1 1 calc R . . H16C H -0.0047 -0.3127 -0.1310 0.077 Uiso 1 1 calc R . . C17 C 0.1264(3) -0.4817(5) -0.0224(3) 0.0592(14) Uani 1 1 d . . . H17A H 0.1795 -0.5218 -0.0163 0.089 Uiso 1 1 calc R . . H17B H 0.0925 -0.4794 -0.0905 0.089 Uiso 1 1 calc R . . H17C H 0.0992 -0.5364 0.0138 0.089 Uiso 1 1 calc R . . C18 C 0.5122(3) -0.0987(4) 0.1612(3) 0.0376(11) Uani 1 1 d . . . C19 C 0.4422(2) -0.1951(4) 0.2994(3) 0.0330(10) Uani 1 1 d . . . C20 C 0.3835(2) 0.0554(5) 0.1839(3) 0.0364(10) Uani 1 1 d . . . C21 C 0.3529(2) -0.1152(4) 0.0121(3) 0.0327(10) Uani 1 1 d . . . C22 C 0.4224(2) -0.3404(5) 0.1285(3) 0.0343(10) Uani 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 Mo 0.02007(19) 0.0274(2) 0.0327(2) -0.00030(16) 0.00329(14) -0.00082(16) Cl 0.0212(5) 0.0273(6) 0.0326(5) 0.0038(4) 0.0013(4) 0.0044(4) P 0.0205(5) 0.0290(7) 0.0278(5) -0.0007(5) 0.0018(4) 0.0001(4) O1 0.0275(15) 0.0331(18) 0.0395(16) -0.0088(13) 0.0103(12) -0.0043(12) O2 0.0325(18) 0.047(2) 0.084(2) 0.0036(17) 0.0214(16) -0.0037(16) O3 0.0353(17) 0.048(2) 0.0380(18) 0.0035(15) 0.0007(14) -0.0013(15) O4 0.0458(19) 0.034(2) 0.065(2) -0.0084(16) 0.0138(16) -0.0046(16) O5 0.0524(19) 0.040(2) 0.0325(17) 0.0034(14) 0.0101(14) 0.0018(15) O6 0.0504(19) 0.039(2) 0.0514(19) -0.0048(16) 0.0046(15) 0.0126(16) C1 0.023(2) 0.031(2) 0.030(2) -0.0034(18) 0.0041(16) 0.0004(18) C2 0.027(2) 0.025(2) 0.035(2) -0.0057(18) 0.0065(17) -0.0056(18) C3 0.0195(19) 0.028(3) 0.036(2) -0.0011(18) 0.0040(16) 0.0005(17) C4 0.026(2) 0.027(2) 0.034(2) -0.0034(18) 0.0076(17) 0.0018(18) C5 0.031(2) 0.033(3) 0.042(2) -0.006(2) 0.0054(19) 0.0028(19) C6 0.037(2) 0.046(3) 0.050(3) -0.020(2) 0.005(2) -0.008(2) C7 0.055(3) 0.028(3) 0.068(3) -0.017(2) 0.024(3) -0.011(2) C8 0.045(3) 0.024(3) 0.062(3) 0.001(2) 0.026(2) 0.005(2) C9 0.028(2) 0.031(3) 0.038(2) -0.0003(19) 0.0104(18) 0.0014(19) C10 0.020(2) 0.029(3) 0.044(3) 0.004(2) 0.0035(18) -0.0005(18) C11 0.027(2) 0.040(3) 0.036(3) -0.004(2) 0.0006(19) -0.003(2) C12 0.029(2) 0.037(3) 0.036(2) -0.012(2) -0.0002(17) -0.007(2) C13 0.035(2) 0.034(3) 0.038(2) 0.002(2) 0.0096(19) -0.001(2) C14 0.035(2) 0.032(3) 0.044(3) -0.001(2) 0.0056(19) -0.003(2) C15 0.027(2) 0.057(3) 0.054(3) 0.002(2) 0.007(2) -0.001(2) C16 0.036(3) 0.066(4) 0.043(3) -0.004(2) 0.001(2) -0.006(2) C17 0.059(3) 0.062(4) 0.051(3) -0.014(3) 0.011(2) -0.009(3) C18 0.029(2) 0.034(3) 0.045(3) 0.001(2) 0.006(2) -0.004(2) C19 0.019(2) 0.032(3) 0.045(3) -0.006(2) 0.0059(18) -0.0050(18) C20 0.025(2) 0.044(3) 0.035(2) -0.002(2) 0.0042(17) -0.002(2) C21 0.026(2) 0.026(3) 0.048(3) -0.003(2) 0.0144(19) -0.0008(18) C22 0.027(2) 0.037(3) 0.031(2) -0.001(2) -0.0011(17) 0.003(2) _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. ; 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 Mo C18 2.012(4) . ? Mo C21 2.028(4) . ? Mo C22 2.030(5) . ? Mo C19 2.045(4) . ? Mo C20 2.067(5) . ? Mo P 2.4686(10) . ? Cl P 2.0765(13) . ? P C1 1.863(4) . ? P C3 1.875(4) . ? O1 C1 1.415(4) . ? O1 C2 1.468(4) . ? O2 C18 1.139(4) . ? O3 C19 1.148(4) . ? O4 C20 1.138(5) . ? O5 C21 1.153(4) . ? O6 C22 1.147(5) . ? C1 C4 1.499(5) . ? C1 H1A 1.0000 . ? C2 C10 1.506(5) . ? C2 C13 1.509(5) . ? C2 C3 1.563(5) . ? C3 C14 1.541(5) . ? C3 C12 1.563(5) . ? C4 C5 1.379(5) . ? C4 C9 1.382(5) . ? C5 C6 1.372(6) . ? C5 H5A 0.9500 . ? C6 C7 1.366(6) . ? C6 H6A 0.9500 . ? C7 C8 1.391(5) . ? C7 H7A 0.9500 . ? C8 C9 1.372(5) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C10 C11 1.327(5) . ? C10 C15 1.501(5) . ? C11 C16 1.497(5) . ? C11 C12 1.512(5) . ? C12 C17 1.515(6) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? 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 C18 Mo C21 92.21(16) . . ? C18 Mo C22 87.80(17) . . ? C21 Mo C22 88.14(15) . . ? C18 Mo C19 89.35(16) . . ? C21 Mo C19 175.20(16) . . ? C22 Mo C19 87.38(15) . . ? C18 Mo C20 87.09(16) . . ? C21 Mo C20 91.60(15) . . ? C22 Mo C20 174.87(16) . . ? C19 Mo C20 93.02(16) . . ? C18 Mo P 171.92(13) . . ? C21 Mo P 87.27(11) . . ? C22 Mo P 100.24(11) . . ? C19 Mo P 91.82(11) . . ? C20 Mo P 84.87(11) . . ? C1 P C3 89.24(17) . . ? C1 P Cl 101.63(13) . . ? C3 P Cl 103.92(12) . . ? C1 P Mo 119.12(11) . . ? C3 P Mo 129.00(12) . . ? Cl P Mo 109.61(5) . . ? C1 O1 C2 113.2(3) . . ? O1 C1 C4 110.8(3) . . ? O1 C1 P 105.3(2) . . ? C4 C1 P 117.1(3) . . ? O1 C1 H1A 107.8 . . ? C4 C1 H1A 107.8 . . ? P C1 H1A 107.8 . . ? O1 C2 C10 107.0(3) . . ? O1 C2 C13 106.3(3) . . ? C10 C2 C13 113.1(3) . . ? O1 C2 C3 111.1(3) . . ? C10 C2 C3 103.6(3) . . ? C13 C2 C3 115.5(3) . . ? C14 C3 C2 115.6(3) . . ? C14 C3 C12 113.7(3) . . ? C2 C3 C12 105.4(3) . . ? C14 C3 P 105.1(2) . . ? C2 C3 P 104.6(2) . . ? C12 C3 P 112.2(3) . . ? C5 C4 C9 118.4(4) . . ? C5 C4 C1 120.3(3) . . ? C9 C4 C1 121.3(3) . . ? C6 C5 C4 121.1(4) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C7 C6 C5 120.4(4) . . ? C7 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? C6 C7 C8 119.1(4) . . ? C6 C7 H7A 120.4 . . ? C8 C7 H7A 120.4 . . ? C9 C8 C7 120.2(4) . . ? C9 C8 H8A 119.9 . . ? C7 C8 H8A 119.9 . . ? C8 C9 C4 120.7(4) . . ? C8 C9 H9A 119.7 . . ? C4 C9 H9A 119.7 . . ? C11 C10 C15 128.4(4) . . ? C11 C10 C2 112.3(3) . . ? C15 C10 C2 119.2(4) . . ? C10 C11 C16 126.4(4) . . ? C10 C11 C12 112.8(3) . . ? C16 C11 C12 120.8(4) . . ? C11 C12 C17 110.5(3) . . ? C11 C12 C3 102.7(3) . . ? C17 C12 C3 116.0(4) . . ? C11 C12 H12A 109.1 . . ? C17 C12 H12A 109.1 . . ? C3 C12 H12A 109.1 . . ? C2 C13 H13A 109.5 . . ? C2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O2 C18 Mo 177.5(4) . . ? O3 C19 Mo 176.0(4) . . ? O4 C20 Mo 176.5(4) . . ? O5 C21 Mo 177.4(3) . . ? O6 C22 Mo 174.7(4) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.964 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.134