# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Hughes, Russell' 'Huang, Hui' 'Rheingold, Arnold' _publ_contact_author_name 'Hughes, Russell' _publ_contact_author_email Russell.P.Hughes@Dartmouth.EDU _publ_section_title ; Synthesis and Structural Characterization of Group 6 Transition Metal Complexes with Terminal Fluoromethylidyne (CF) Ligands; a DFT/NBO/NRT Comparison of Bonding Characteristics of Terminal NO, CF and CH Ligands. ; # Attachment '- allRPH.cif' data_rph438 _database_code_depnum_ccdc_archive 'CCDC 793583' #TrackingRef '- allRPH.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H5 F O2 W' _chemical_formula_weight 335.97 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 5.8048(4) _cell_length_b 19.8293(12) _cell_length_c 7.0601(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.3340(10) _cell_angle_gamma 90.00 _cell_volume 809.13(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 289 _cell_measurement_theta_min 5.35 _cell_measurement_theta_max 23.23 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 14.243 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.434 _exptl_absorpt_correction_T_max 0.736 _exptl_absorpt_process_details sadabs _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 'CCD detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 7596 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 28.21 _reflns_number_total 1866 _reflns_number_gt 1658 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0080P)^2^+2.8153P] 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 1866 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0257 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0387 _refine_ls_wR_factor_gt 0.0371 _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 -0.1440(7) 0.4371(2) 0.7430(6) 0.0223(9) Uani 1 1 d . . . H1 H -0.2680 0.4485 0.8112 0.027 Uiso 1 1 calc R . . C2 C 0.0602(7) 0.4737(2) 0.7399(6) 0.0212(9) Uani 1 1 d . . . H2 H 0.0954 0.5135 0.8060 0.025 Uiso 1 1 calc R . . C3 C 0.2047(8) 0.4406(2) 0.6204(6) 0.0248(9) Uani 1 1 d . . . H3 H 0.3507 0.4547 0.5931 0.030 Uiso 1 1 calc R . . C4 C 0.0877(9) 0.3820(2) 0.5494(6) 0.0289(11) Uani 1 1 d . . . H4 H 0.1446 0.3506 0.4676 0.035 Uiso 1 1 calc R . . C5 C -0.1310(8) 0.3791(2) 0.6236(6) 0.0258(10) Uani 1 1 d . . . H5 H -0.2436 0.3460 0.5996 0.031 Uiso 1 1 calc R . . C6 C 0.3431(7) 0.2886(2) 0.8736(5) 0.0194(8) Uani 1 1 d . . . C7 C 0.3657(7) 0.4010(2) 1.0873(5) 0.0199(9) Uani 1 1 d . . . C8 C -0.0257(7) 0.3237(2) 1.0584(5) 0.0190(8) Uani 1 1 d . . . O1 O 0.4594(5) 0.23819(14) 0.8686(4) 0.0307(7) Uani 0.67 1 d P A 1 F1A F 0.4594(5) 0.23819(14) 0.8686(4) 0.0307(7) Uani 0.33 1 d P A 2 O2 O 0.4985(5) 0.42168(15) 1.2175(4) 0.0327(7) Uani 0.67 1 d P A 1 F1B F 0.4985(5) 0.42168(15) 1.2175(4) 0.0327(7) Uani 0.33 1 d P A 2 F1 F -0.1453(5) 0.29653(15) 1.1649(4) 0.0314(7) Uani 0.33 1 d P A 1 O3 O -0.1453(5) 0.29653(15) 1.1649(4) 0.0314(7) Uani 0.67 1 d P A 2 W1 W 0.15746(3) 0.368731(8) 0.88166(2) 0.01924(6) Uani 1 1 d . A . 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 0.016(2) 0.026(2) 0.024(2) 0.0067(17) 0.0016(17) 0.0069(18) C2 0.023(2) 0.017(2) 0.022(2) 0.0026(16) -0.0030(17) 0.0009(17) C3 0.021(2) 0.029(2) 0.023(2) 0.0102(17) -0.0004(18) -0.0001(19) C4 0.041(3) 0.030(3) 0.0147(19) -0.0002(16) -0.0021(18) 0.015(2) C5 0.026(2) 0.025(2) 0.025(2) 0.0057(17) -0.0104(18) -0.0062(18) C6 0.020(2) 0.022(2) 0.0167(18) -0.0011(15) 0.0028(16) -0.0032(17) C7 0.021(2) 0.016(2) 0.023(2) 0.0020(16) 0.0023(17) 0.0020(17) C8 0.015(2) 0.020(2) 0.0208(19) -0.0012(16) -0.0029(16) 0.0027(17) O1 0.0325(18) 0.0245(16) 0.0360(16) -0.0040(12) 0.0089(14) 0.0049(14) F1A 0.0325(18) 0.0245(16) 0.0360(16) -0.0040(12) 0.0089(14) 0.0049(14) O2 0.0234(17) 0.0365(17) 0.0372(16) -0.0144(14) -0.0026(13) -0.0069(14) F1B 0.0234(17) 0.0365(17) 0.0372(16) -0.0144(14) -0.0026(13) -0.0069(14) F1 0.0244(17) 0.0320(17) 0.0389(17) 0.0073(13) 0.0085(14) -0.0051(13) O3 0.0244(17) 0.0320(17) 0.0389(17) 0.0073(13) 0.0085(14) -0.0051(13) W1 0.01928(10) 0.01946(9) 0.01829(8) 0.00475(7) -0.00190(6) 0.00182(7) _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 1.391(6) . ? C1 C5 1.433(6) . ? C1 W1 2.354(4) . ? C1 H1 0.9300 . ? C2 C3 1.406(6) . ? C2 W1 2.355(4) . ? C2 H2 0.9300 . ? C3 C4 1.414(6) . ? C3 W1 2.367(4) . ? C3 H3 0.9300 . ? C4 C5 1.419(7) . ? C4 W1 2.358(4) . ? C4 H4 0.9300 . ? C5 W1 2.366(4) . ? C5 H5 0.9300 . ? C6 O1 1.208(5) . ? C6 W1 1.924(4) . ? C7 O2 1.215(5) . ? C7 W1 1.911(4) . ? C8 F1 1.198(5) . ? C8 W1 1.932(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 C2 C1 C5 108.5(4) . . ? C2 C1 W1 72.9(2) . . ? C5 C1 W1 72.8(2) . . ? C2 C1 H1 125.7 . . ? C5 C1 H1 125.7 . . ? W1 C1 H1 120.4 . . ? C1 C2 C3 108.9(4) . . ? C1 C2 W1 72.8(2) . . ? C3 C2 W1 73.1(2) . . ? C1 C2 H2 125.6 . . ? C3 C2 H2 125.6 . . ? W1 C2 H2 120.3 . . ? C2 C3 C4 107.6(4) . . ? C2 C3 W1 72.2(2) . . ? C4 C3 W1 72.3(2) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? W1 C3 H3 121.1 . . ? C3 C4 C5 108.6(4) . . ? C3 C4 W1 72.9(2) . . ? C5 C4 W1 72.8(2) . . ? C3 C4 H4 125.7 . . ? C5 C4 H4 125.7 . . ? W1 C4 H4 120.3 . . ? C4 C5 C1 106.4(4) . . ? C4 C5 W1 72.2(2) . . ? C1 C5 W1 71.9(2) . . ? C4 C5 H5 126.8 . . ? C1 C5 H5 126.8 . . ? W1 C5 H5 121.0 . . ? O1 C6 W1 179.9(4) . . ? O2 C7 W1 179.7(4) . . ? F1 C8 W1 178.0(3) . . ? C7 W1 C6 89.01(17) . . ? C7 W1 C8 90.66(17) . . ? C6 W1 C8 88.89(17) . . ? C7 W1 C1 121.06(16) . . ? C6 W1 C1 149.37(15) . . ? C8 W1 C1 95.89(16) . . ? C7 W1 C2 97.84(16) . . ? C6 W1 C2 146.11(16) . . ? C8 W1 C2 123.96(16) . . ? C1 W1 C2 34.36(14) . . ? C7 W1 C4 139.14(17) . . ? C6 W1 C4 96.17(15) . . ? C8 W1 C4 129.81(17) . . ? C1 W1 C4 57.98(15) . . ? C2 W1 C4 57.75(14) . . ? C7 W1 C5 155.27(16) . . ? C6 W1 C5 114.03(16) . . ? C8 W1 C5 98.32(16) . . ? C1 W1 C5 35.35(15) . . ? C2 W1 C5 58.11(14) . . ? C4 W1 C5 34.97(16) . . ? C7 W1 C3 106.22(16) . . ? C6 W1 C3 111.62(16) . . ? C8 W1 C3 153.16(16) . . ? C1 W1 C3 57.62(15) . . ? C2 W1 C3 34.64(15) . . ? C4 W1 C3 34.83(15) . . ? C5 W1 C3 58.18(15) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.620 _refine_diff_density_min -1.999 _refine_diff_density_rms 0.152 #===END data_rph387 _database_code_depnum_ccdc_archive 'CCDC 793584' #TrackingRef '- allRPH.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H15 F O2 W' _chemical_formula_weight 406.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 6.9376(10) _cell_length_b 12.5405(18) _cell_length_c 7.7025(11) _cell_angle_alpha 90.00 _cell_angle_beta 101.873(2) _cell_angle_gamma 90.00 _cell_volume 655.79(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4687 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 28.17 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.057 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 384 _exptl_absorpt_coefficient_mu 8.806 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2719 _exptl_absorpt_correction_T_max 0.4730 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 5584 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 28.18 _reflns_number_total 1587 _reflns_number_gt 1511 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0200P)^2^+1.3000P] 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 1587 _refine_ls_number_parameters 92 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0206 _refine_ls_R_factor_gt 0.0193 _refine_ls_wR_factor_ref 0.0466 _refine_ls_wR_factor_gt 0.0458 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.006 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 W1 W 0.49323(2) 0.2500 0.29800(2) 0.03321(8) Uani 1 2 d S . . 02 O 0.6568(4) 0.0752(2) 0.0754(3) 0.060(10) Uani 0.50 1 d P . . F1 F 0.6568(4) 0.0752(2) 0.0754(3) 0.046(7) Uani 0.50 1 d P . . O1 O 0.8760(5) 0.2500 0.5933(5) 0.0481(10) Uani 1 2 d S . . C1 C 0.2896(4) 0.1934(3) 0.4903(4) 0.0310(7) Uani 1 1 d . . . C2 C 0.2009(4) 0.1582(3) 0.3168(4) 0.0302(6) Uani 1 1 d . . . C3 C 0.1484(6) 0.2500 0.2088(5) 0.0292(9) Uani 1 2 d S . . C4 C 0.3496(6) 0.1249(4) 0.6516(6) 0.0628(14) Uani 1 1 d . . . H7A H 0.2364 0.1138 0.7074 0.094 Uiso 1 1 calc R . . H7B H 0.4556 0.1601 0.7358 0.094 Uiso 1 1 calc R . . H7C H 0.3962 0.0558 0.6171 0.094 Uiso 1 1 calc R . . C5 C 0.1535(6) 0.0447(3) 0.2626(8) 0.0644(14) Uani 1 1 d . . . H6A H 0.0232 0.0263 0.2843 0.097 Uiso 1 1 calc R . . H6B H 0.2528 -0.0026 0.3319 0.097 Uiso 1 1 calc R . . H6C H 0.1536 0.0364 0.1361 0.097 Uiso 1 1 calc R . . C6 C 0.0377(7) 0.2500 0.0190(7) 0.0586(18) Uani 1 2 d S . . H10A H -0.1042 0.2500 0.0158 0.088 Uiso 1 2 calc SR . . H10B H 0.0727 0.1862 -0.0412 0.088 Uiso 1 1 calc R . . C7 C 0.5936(5) 0.1436(3) 0.1639(4) 0.0334(7) Uani 1 1 d . . . C8 C 0.7362(6) 0.2500 0.4803(6) 0.0325(10) Uani 1 2 d S . . 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 W1 0.01279(9) 0.06857(15) 0.01882(10) 0.000 0.00452(6) 0.000 02 0.043(16) 0.081(18) 0.054(15) -0.003(12) 0.010(10) -0.011(13) F1 0.058(13) 0.053(11) 0.036(9) -0.027(8) 0.027(8) -0.017(9) O1 0.0244(17) 0.090(3) 0.0269(17) 0.000 -0.0014(13) 0.000 C1 0.0157(13) 0.0535(18) 0.0260(14) 0.0088(13) 0.0093(11) 0.0044(12) C2 0.0158(13) 0.0397(17) 0.0377(16) -0.0053(13) 0.0116(11) 0.0004(12) C3 0.0141(18) 0.055(3) 0.0195(18) 0.000 0.0054(14) 0.000 C4 0.037(2) 0.107(4) 0.049(2) 0.044(3) 0.0188(17) 0.023(2) C5 0.033(2) 0.050(2) 0.116(4) -0.033(3) 0.028(2) -0.0065(17) C6 0.020(2) 0.132(6) 0.022(2) 0.000 0.0017(18) 0.000 C7 0.0217(15) 0.0498(19) 0.0302(16) -0.0066(14) 0.0089(12) -0.0073(14) C8 0.020(2) 0.054(3) 0.025(2) 0.000 0.0093(16) 0.000 _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 W1 C7 1.905(4) 4_565 ? W1 C7 1.905(4) . ? W1 C8 1.959(4) . ? W1 C3 2.349(4) . ? W1 C1 2.357(3) 4_565 ? W1 C1 2.357(3) . ? W1 C2 2.362(3) 4_565 ? W1 C2 2.362(3) . ? 02 C7 1.231(4) . ? F1 C7 1.231(4) . ? O1 C8 1.162(6) . ? C1 C1 1.420(7) 4_565 ? C1 C2 1.421(4) . ? C1 C4 1.497(5) . ? C2 C3 1.423(4) . ? C2 C5 1.501(5) . ? C3 C2 1.423(4) 4_565 ? C3 C6 1.505(6) . ? C4 H7A 0.9800 . ? C4 H7B 0.9800 . ? C4 H7C 0.9800 . ? C5 H6A 0.9800 . ? C5 H6B 0.9800 . ? C5 H6C 0.9800 . ? C6 H10A 0.9800 . ? C6 H10B 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 C7 W1 C7 89.0(2) 4_565 . ? C7 W1 C8 91.82(13) 4_565 . ? C7 W1 C8 91.82(13) . . ? C7 W1 C3 107.78(11) 4_565 . ? C7 W1 C3 107.78(11) . . ? C8 W1 C3 152.11(16) . . ? C7 W1 C1 117.59(13) 4_565 4_565 ? C7 W1 C1 152.25(13) . 4_565 ? C8 W1 C1 95.07(14) . 4_565 ? C3 W1 C1 58.52(11) . 4_565 ? C7 W1 C1 152.25(13) 4_565 . ? C7 W1 C1 117.58(13) . . ? C8 W1 C1 95.07(14) . . ? C3 W1 C1 58.53(11) . . ? C1 W1 C1 35.05(17) 4_565 . ? C7 W1 C2 96.10(12) 4_565 4_565 ? C7 W1 C2 142.09(12) . 4_565 ? C8 W1 C2 125.38(13) . 4_565 ? C3 W1 C2 35.16(9) . 4_565 ? C1 W1 C2 35.06(11) 4_565 4_565 ? C1 W1 C2 58.32(11) . 4_565 ? C7 W1 C2 142.09(12) 4_565 . ? C7 W1 C2 96.10(12) . . ? C8 W1 C2 125.38(13) . . ? C3 W1 C2 35.16(9) . . ? C1 W1 C2 58.32(11) 4_565 . ? C1 W1 C2 35.06(11) . . ? C2 W1 C2 58.31(15) 4_565 . ? C1 C1 C2 108.07(19) 4_565 . ? C1 C1 C4 125.0(3) 4_565 . ? C2 C1 C4 126.5(4) . . ? C1 C1 W1 72.47(9) 4_565 . ? C2 C1 W1 72.65(16) . . ? C4 C1 W1 126.4(2) . . ? C1 C2 C3 108.0(3) . . ? C1 C2 C5 125.7(4) . . ? C3 C2 C5 126.1(3) . . ? C1 C2 W1 72.30(16) . . ? C3 C2 W1 71.9(2) . . ? C5 C2 W1 125.9(2) . . ? C2 C3 C2 107.9(4) 4_565 . ? C2 C3 C6 125.89(18) 4_565 . ? C2 C3 C6 125.89(18) . . ? C2 C3 W1 72.91(19) 4_565 . ? C2 C3 W1 72.91(19) . . ? C6 C3 W1 124.7(3) . . ? C1 C4 H7A 109.5 . . ? C1 C4 H7B 109.5 . . ? H7A C4 H7B 109.5 . . ? C1 C4 H7C 109.5 . . ? H7A C4 H7C 109.5 . . ? H7B C4 H7C 109.5 . . ? C2 C5 H6A 109.5 . . ? C2 C5 H6B 109.5 . . ? H6A C5 H6B 109.5 . . ? C2 C5 H6C 109.5 . . ? H6A C5 H6C 109.5 . . ? H6B C5 H6C 109.5 . . ? C3 C6 H10A 109.5 . . ? C3 C6 H10B 109.5 . . ? H10A C6 H10B 109.5 . . ? F1 C7 02 0.0(2) . . ? F1 C7 W1 179.2(3) . . ? 02 C7 W1 179.2(3) . . ? O1 C8 W1 177.4(4) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.201 _refine_diff_density_min -1.375 _refine_diff_density_rms 0.100 #===END data_rph381a _database_code_depnum_ccdc_archive 'CCDC 793585' #TrackingRef '- allRPH.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H5 Co2 F Mo O8' _chemical_formula_weight 533.98 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 19.664(5) _cell_length_b 8.982(2) _cell_length_c 19.389(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3424.5(14) _cell_formula_units_Z 8 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 6070 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.12 _exptl_crystal_description block _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 2.686 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4996 _exptl_absorpt_correction_T_max 0.6157 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 17172 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.17 _reflns_number_total 6732 _reflns_number_gt 6430 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0400P)^2^+0.0200P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.073(13) _refine_ls_number_reflns 6732 _refine_ls_number_parameters 469 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Mo1 Mo 0.484100(15) 0.57608(4) 0.27650(2) 0.02650(9) Uani 1 1 d . . . Mo1' Mo 0.246381(17) 1.05131(4) -0.01429(2) 0.03010(10) Uani 1 1 d . . . Co1' Co 0.32899(3) 0.80533(6) 0.00030(4) 0.02897(14) Uani 1 1 d . . . Co1 Co 0.61335(3) 0.59253(6) 0.22389(4) 0.02788(14) Uani 1 1 d . . . Co2' Co 0.37500(3) 1.05074(6) 0.04002(4) 0.03154(15) Uani 1 1 d . . . Co2 Co 0.56956(2) 0.33888(6) 0.25299(4) 0.02933(15) Uani 1 1 d . . . F1 F 0.60969(13) 0.5226(3) 0.36947(16) 0.0363(6) Uani 1 1 d . . . F1' F 0.37202(12) 1.0066(3) -0.10801(16) 0.0400(7) Uani 1 1 d . . . O6 O 0.39511(19) 0.3229(5) 0.2141(4) 0.097(2) Uani 1 1 d . . . O7 O 0.4736(3) 0.7211(7) 0.1313(3) 0.0813(17) Uani 1 1 d . . . O7' O 0.2336(3) 1.1599(7) 0.1368(3) 0.099(2) Uani 1 1 d . . . O6' O 0.1561(2) 0.7873(5) 0.0338(5) 0.130(3) Uani 1 1 d . . . O9 O 0.6053(2) 0.9150(4) 0.2392(3) 0.0659(13) Uani 1 1 d . . . O9' O 0.25599(19) 0.6270(4) -0.1012(3) 0.0588(12) Uani 1 1 d . . . O10 O 0.6131(3) 0.5562(5) 0.0723(3) 0.0697(14) Uani 1 1 d . . . O10' O 0.2911(3) 0.6713(6) 0.1338(3) 0.0917(18) Uani 1 1 d . . . O11 O 0.75751(16) 0.5519(4) 0.2581(3) 0.0517(12) Uani 1 1 d . . . O11' O 0.46378(17) 0.6759(4) -0.0222(2) 0.0507(10) Uani 1 1 d . . . O12 O 0.4958(2) 0.1405(5) 0.3459(3) 0.0611(12) Uani 1 1 d . . . O12' O 0.3743(3) 1.3756(4) 0.0333(3) 0.0739(15) Uani 1 1 d . . . O13 O 0.70350(16) 0.1991(4) 0.2636(3) 0.0641(14) Uani 1 1 d . . . O13' O 0.3679(3) 0.9846(5) 0.1897(3) 0.0732(14) Uani 1 1 d . . . O14' O 0.51874(16) 1.0033(5) 0.0072(3) 0.0651(14) Uani 1 1 d . . . O14 O 0.5252(2) 0.2529(7) 0.1128(3) 0.091(2) Uani 1 1 d . . . C1 C 0.4414(2) 0.7982(5) 0.3162(3) 0.0380(11) Uani 1 1 d . . . H1A H 0.4433 0.8945 0.2914 0.046 Uiso 1 1 calc R . . C1' C 0.1535(2) 1.1892(6) -0.0481(4) 0.0473(14) Uani 1 1 d . . . H1'A H 0.1117 1.2052 -0.0205 0.057 Uiso 1 1 calc R . . C2 C 0.4877(2) 0.7502(6) 0.3670(3) 0.0438(13) Uani 1 1 d . . . H2A H 0.5284 0.8051 0.3832 0.053 Uiso 1 1 calc R . . C2' C 0.1623(3) 1.0809(6) -0.0982(4) 0.0599(19) Uani 1 1 d . . . H2'A H 0.1283 1.0051 -0.1119 0.072 Uiso 1 1 calc R . . C3 C 0.4628(3) 0.6164(7) 0.3941(3) 0.0515(15) Uani 1 1 d . . . H3A H 0.4834 0.5598 0.4326 0.062 Uiso 1 1 calc R . . C3' C 0.2254(3) 1.1071(7) -0.1308(3) 0.0595(17) Uani 1 1 d . . . H3'A H 0.2437 1.0521 -0.1710 0.071 Uiso 1 1 calc R . . C4' C 0.2547(3) 1.2337(7) -0.1003(4) 0.0494(15) Uani 1 1 d . . . H4'A H 0.2970 1.2836 -0.1155 0.059 Uiso 1 1 calc R . . C4 C 0.4011(3) 0.5824(6) 0.3617(4) 0.0516(16) Uani 1 1 d . . . H4A H 0.3700 0.4999 0.3742 0.062 Uiso 1 1 calc R . . C5 C 0.3874(2) 0.6974(6) 0.3140(3) 0.0427(13) Uani 1 1 d . . . H5A H 0.3448 0.7098 0.2874 0.051 Uiso 1 1 calc R . . C5' C 0.2105(2) 1.2843(5) -0.0494(4) 0.0456(14) Uani 1 1 d . . . H5'A H 0.2156 1.3778 -0.0229 0.055 Uiso 1 1 calc R . . C6 C 0.4307(2) 0.4112(6) 0.2355(4) 0.0591(19) Uani 1 1 d . . . C6' C 0.1922(3) 0.8790(6) 0.0181(5) 0.076(3) Uani 1 1 d . . . C7' C 0.2422(3) 1.1166(8) 0.0823(4) 0.0582(17) Uani 1 1 d . . . C7 C 0.4816(3) 0.6612(7) 0.1832(4) 0.0527(16) Uani 1 1 d . . . C8' C 0.34109(18) 0.9864(4) -0.0458(3) 0.0274(9) Uani 1 1 d . . . C8 C 0.58029(19) 0.5114(5) 0.3067(3) 0.0279(10) Uani 1 1 d . . . C9' C 0.2842(2) 0.6957(5) -0.0616(3) 0.0392(12) Uani 1 1 d . . . C9 C 0.6094(2) 0.7910(5) 0.2341(3) 0.0406(12) Uani 1 1 d . . . C10 C 0.6126(3) 0.5714(6) 0.1299(3) 0.0433(13) Uani 1 1 d . . . C10' C 0.3049(3) 0.7213(6) 0.0828(4) 0.0520(15) Uani 1 1 d . . . C11 C 0.7022(2) 0.5655(5) 0.2443(3) 0.0358(11) Uani 1 1 d . . . C11' C 0.4114(2) 0.7241(5) -0.0131(3) 0.0356(11) Uani 1 1 d . . . C12 C 0.5248(2) 0.2168(5) 0.3097(4) 0.0423(13) Uani 1 1 d . . . C12' C 0.3746(3) 1.2504(6) 0.0369(3) 0.0451(13) Uani 1 1 d . . . C13 C 0.6520(2) 0.2540(5) 0.2589(3) 0.0430(14) Uani 1 1 d . . . C13' C 0.3701(3) 1.0128(6) 0.1330(4) 0.0500(15) Uani 1 1 d . . . C14' C 0.4638(2) 1.0197(6) 0.0207(3) 0.0417(13) Uani 1 1 d . . . C14 C 0.5425(2) 0.2822(6) 0.1670(4) 0.0499(15) 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 Mo1 0.02161(14) 0.02467(16) 0.0332(2) -0.00402(16) 0.00030(15) 0.00236(12) Mo1' 0.02360(15) 0.02455(16) 0.0421(3) 0.00193(17) 0.00334(16) 0.00237(13) Co1' 0.0313(3) 0.0214(3) 0.0343(4) 0.0001(2) 0.0020(3) 0.00243(19) Co1 0.0283(2) 0.0242(3) 0.0311(4) 0.0003(3) 0.0058(2) -0.00182(19) Co2' 0.0309(3) 0.0247(3) 0.0390(4) -0.0035(3) -0.0032(3) 0.0029(2) Co2 0.0247(2) 0.0202(3) 0.0431(4) -0.0048(2) 0.0041(2) -0.00100(18) F1 0.0362(12) 0.0438(16) 0.0290(18) -0.0017(13) -0.0033(12) -0.0003(11) F1' 0.0397(14) 0.0460(16) 0.0343(19) 0.0084(14) 0.0103(12) 0.0024(12) O6 0.0335(18) 0.080(3) 0.176(7) -0.074(4) -0.012(3) -0.0016(19) O7 0.079(3) 0.127(5) 0.038(3) 0.019(3) -0.002(2) 0.046(3) O7' 0.092(4) 0.155(6) 0.050(4) -0.019(4) 0.012(3) 0.061(4) O6' 0.057(3) 0.057(3) 0.276(10) 0.048(4) 0.074(4) -0.002(2) O9 0.090(3) 0.0266(19) 0.082(4) -0.001(2) 0.020(3) 0.0004(17) O9' 0.0460(19) 0.054(2) 0.077(4) -0.014(2) -0.012(2) -0.0072(18) O10 0.101(4) 0.079(3) 0.030(3) -0.002(2) 0.014(3) 0.001(3) O10' 0.137(5) 0.078(4) 0.059(4) 0.028(3) 0.033(4) -0.002(3) O11 0.0308(16) 0.060(2) 0.064(4) -0.003(2) 0.0017(17) -0.0032(13) O11' 0.0398(17) 0.048(2) 0.064(3) -0.014(2) -0.0072(18) 0.0146(14) O12 0.056(2) 0.050(2) 0.078(4) 0.013(2) 0.009(2) -0.0148(19) O12' 0.098(3) 0.031(2) 0.093(4) -0.003(2) -0.014(3) -0.004(2) O13 0.0337(17) 0.045(2) 0.113(5) 0.006(2) 0.006(2) 0.0109(14) O13' 0.112(4) 0.069(3) 0.038(3) 0.005(2) -0.012(3) 0.027(3) O14' 0.0359(18) 0.064(3) 0.095(4) -0.029(3) -0.002(2) 0.0044(17) O14 0.062(3) 0.134(5) 0.078(4) -0.058(4) 0.003(3) -0.021(3) C1 0.040(2) 0.030(2) 0.044(3) -0.005(2) 0.007(2) 0.0109(18) C1' 0.035(2) 0.042(3) 0.065(5) -0.001(3) -0.013(3) 0.0089(19) C2 0.040(2) 0.051(3) 0.040(4) -0.016(3) 0.003(2) 0.006(2) C2' 0.039(3) 0.055(3) 0.086(6) -0.012(3) -0.032(3) 0.005(2) C3 0.060(3) 0.061(4) 0.034(4) 0.005(3) 0.008(3) 0.028(3) C3' 0.076(4) 0.070(4) 0.032(4) 0.000(3) -0.013(3) 0.028(3) C4' 0.043(3) 0.054(3) 0.051(4) 0.020(3) -0.006(3) 0.007(2) C4 0.048(3) 0.040(3) 0.067(5) 0.004(3) 0.030(3) 0.005(2) C5 0.026(2) 0.045(3) 0.057(4) -0.009(3) 0.005(2) 0.0129(18) C5' 0.045(3) 0.032(3) 0.060(4) 0.007(2) -0.009(3) 0.0063(19) C6 0.025(2) 0.048(3) 0.105(6) -0.034(4) -0.004(3) 0.0011(18) C6' 0.037(3) 0.039(3) 0.152(8) 0.017(4) 0.034(4) 0.009(2) C7' 0.048(3) 0.078(4) 0.049(5) -0.004(4) 0.011(3) 0.034(3) C7 0.043(3) 0.069(4) 0.046(5) 0.002(3) 0.003(3) 0.019(2) C8' 0.0265(17) 0.0200(19) 0.036(3) 0.0015(18) 0.0018(18) -0.0011(14) C8 0.0255(18) 0.025(2) 0.034(3) -0.0042(19) 0.0031(17) -0.0012(15) C9' 0.030(2) 0.030(2) 0.058(4) -0.001(2) -0.001(2) -0.0005(17) C9 0.048(2) 0.031(2) 0.042(4) 0.002(2) 0.007(2) -0.0025(18) C10 0.045(3) 0.042(3) 0.042(4) -0.005(2) 0.008(2) 0.000(2) C10' 0.059(3) 0.033(3) 0.064(5) 0.009(3) 0.012(3) 0.000(2) C11 0.032(2) 0.034(2) 0.041(3) -0.002(2) 0.008(2) -0.0076(16) C11' 0.041(2) 0.032(2) 0.034(3) -0.008(2) -0.006(2) 0.0011(17) C12 0.038(2) 0.023(2) 0.066(4) 0.000(2) 0.008(2) -0.0033(18) C12' 0.050(3) 0.037(3) 0.049(4) -0.005(3) -0.007(2) 0.001(2) C13 0.033(2) 0.028(2) 0.068(5) 0.004(2) 0.013(2) -0.0033(17) C13' 0.060(3) 0.038(3) 0.052(5) -0.004(3) -0.018(3) 0.011(2) C14' 0.036(2) 0.031(2) 0.057(4) -0.011(2) -0.006(2) 0.0002(19) C14 0.033(2) 0.050(3) 0.067(5) -0.026(3) 0.009(3) -0.006(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 Mo1 C7 1.965(7) . ? Mo1 C6 1.982(5) . ? Mo1 C8 2.063(4) . ? Mo1 C1 2.298(4) . ? Mo1 C5 2.309(4) . ? Mo1 C4 2.323(5) . ? Mo1 C3 2.345(6) . ? Mo1 C2 2.352(6) . ? Mo1 Co1 2.7426(8) . ? Mo1 Co2 2.7516(8) . ? Mo1' C7' 1.963(7) . ? Mo1' C6' 1.982(6) . ? Mo1' C8' 2.045(4) . ? Mo1' C1' 2.302(5) . ? Mo1' C5' 2.311(5) . ? Mo1' C2' 2.335(6) . ? Mo1' C4' 2.344(6) . ? Mo1' C3' 2.350(7) . ? Mo1' Co2' 2.7396(9) . ? Mo1' Co1' 2.7568(8) . ? Co1' C9' 1.785(5) . ? Co1' C11' 1.795(4) . ? Co1' C10' 1.832(7) . ? Co1' C8' 1.871(4) . ? Co1' Co2' 2.5041(9) . ? Co1 C9 1.795(5) . ? Co1 C11 1.808(4) . ? Co1 C10 1.833(7) . ? Co1 C8 1.879(5) . ? Co1 Co2 2.5001(9) . ? Co2' C12' 1.794(5) . ? Co2' C14' 1.807(5) . ? Co2' C13' 1.838(7) . ? Co2' C8' 1.884(5) . ? Co2 C12 1.785(5) . ? Co2 C13 1.795(4) . ? Co2 C14 1.822(7) . ? Co2 C8 1.879(4) . ? F1 C8 1.352(5) . ? F1' C8' 1.363(5) . ? O6 C6 1.136(6) . ? O7 C7 1.152(8) . ? O7' C7' 1.140(9) . ? O6' C6' 1.129(7) . ? O9 C9 1.121(5) . ? O9' C9' 1.131(7) . ? O10 C10 1.125(8) . ? O10' C10' 1.119(8) . ? O11 C11 1.127(5) . ? O11' C11' 1.132(5) . ? O12 C12 1.133(7) . ? O12' C12' 1.127(6) . ? O13 C13 1.130(5) . ? O13' C13' 1.127(8) . ? O14' C14' 1.122(6) . ? O14 C14 1.135(9) . ? C1 C5 1.397(7) . ? C1 C2 1.410(8) . ? C1 H1A 0.9900 . ? C1' C2' 1.386(9) . ? C1' C5' 1.410(7) . ? C1' H1'A 0.9900 . ? C2 C3 1.400(9) . ? C2 H2A 0.9900 . ? C2' C3' 1.414(10) . ? C2' H2'A 0.9900 . ? C3 C4 1.400(9) . ? C3 H3A 0.9900 . ? C3' C4' 1.404(9) . ? C3' H3'A 0.9900 . ? C4' C5' 1.391(9) . ? C4' H4'A 0.9900 . ? C4 C5 1.413(8) . ? C4 H4A 0.9900 . ? C5 H5A 0.9900 . ? C5' H5'A 0.9900 . ? 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 C7 Mo1 C6 84.7(3) . . ? C7 Mo1 C8 113.15(19) . . ? C6 Mo1 C8 112.89(18) . . ? C7 Mo1 C1 87.8(2) . . ? C6 Mo1 C1 126.14(18) . . ? C8 Mo1 C1 118.99(18) . . ? C7 Mo1 C5 94.9(2) . . ? C6 Mo1 C5 92.44(19) . . ? C8 Mo1 C5 143.0(2) . . ? C1 Mo1 C5 35.29(17) . . ? C7 Mo1 C4 128.9(2) . . ? C6 Mo1 C4 86.1(3) . . ? C8 Mo1 C4 116.7(2) . . ? C1 Mo1 C4 58.92(19) . . ? C5 Mo1 C4 35.5(2) . . ? C7 Mo1 C3 146.1(2) . . ? C6 Mo1 C3 114.3(3) . . ? C8 Mo1 C3 86.07(19) . . ? C1 Mo1 C3 58.3(2) . . ? C5 Mo1 C3 58.3(2) . . ? C4 Mo1 C3 34.9(2) . . ? C7 Mo1 C2 115.4(3) . . ? C6 Mo1 C2 144.3(2) . . ? C8 Mo1 C2 87.02(18) . . ? C1 Mo1 C2 35.3(2) . . ? C5 Mo1 C2 58.42(18) . . ? C4 Mo1 C2 58.3(2) . . ? C3 Mo1 C2 34.7(2) . . ? C7 Mo1 Co1 70.08(15) . . ? C6 Mo1 Co1 112.44(17) . . ? C8 Mo1 Co1 43.21(13) . . ? C1 Mo1 Co1 114.63(12) . . ? C5 Mo1 Co1 148.75(13) . . ? C4 Mo1 Co1 156.11(18) . . ? C3 Mo1 Co1 121.23(15) . . ? C2 Mo1 Co1 102.35(13) . . ? C7 Mo1 Co2 99.42(16) . . ? C6 Mo1 Co2 71.23(13) . . ? C8 Mo1 Co2 43.04(12) . . ? C1 Mo1 Co2 162.03(13) . . ? C5 Mo1 Co2 156.99(14) . . ? C4 Mo1 Co2 124.45(14) . . ? C3 Mo1 Co2 112.92(13) . . ? C2 Mo1 Co2 128.33(13) . . ? Co1 Mo1 Co2 54.14(2) . . ? C7' Mo1' C6' 84.7(3) . . ? C7' Mo1' C8' 114.1(2) . . ? C6' Mo1' C8' 111.22(19) . . ? C7' Mo1' C1' 94.5(2) . . ? C6' Mo1' C1' 94.8(2) . . ? C8' Mo1' C1' 142.3(2) . . ? C7' Mo1' C5' 89.9(2) . . ? C6' Mo1' C5' 129.6(2) . . ? C8' Mo1' C5' 116.61(18) . . ? C1' Mo1' C5' 35.59(17) . . ? C7' Mo1' C2' 126.9(2) . . ? C6' Mo1' C2' 85.9(3) . . ? C8' Mo1' C2' 118.0(2) . . ? C1' Mo1' C2' 34.8(2) . . ? C5' Mo1' C2' 58.4(2) . . ? C7' Mo1' C4' 118.2(3) . . ? C6' Mo1' C4' 144.0(3) . . ? C8' Mo1' C4' 85.60(19) . . ? C1' Mo1' C4' 58.4(2) . . ? C5' Mo1' C4' 34.8(2) . . ? C2' Mo1' C4' 58.3(2) . . ? C7' Mo1' C3' 147.7(2) . . ? C6' Mo1' C3' 112.2(3) . . ? C8' Mo1' C3' 86.2(2) . . ? C1' Mo1' C3' 58.2(2) . . ? C5' Mo1' C3' 58.0(2) . . ? C2' Mo1' C3' 35.1(3) . . ? C4' Mo1' C3' 34.8(2) . . ? C7' Mo1' Co2' 70.87(16) . . ? C6' Mo1' Co2' 111.9(2) . . ? C8' Mo1' Co2' 43.41(14) . . ? C1' Mo1' Co2' 147.43(13) . . ? C5' Mo1' Co2' 113.36(13) . . ? C2' Mo1' Co2' 157.2(2) . . ? C4' Mo1' Co2' 102.17(14) . . ? C3' Mo1' Co2' 122.11(18) . . ? C7' Mo1' Co1' 99.55(17) . . ? C6' Mo1' Co1' 70.03(15) . . ? C8' Mo1' Co1' 42.74(12) . . ? C1' Mo1' Co1' 158.12(14) . . ? C5' Mo1' Co1' 159.34(14) . . ? C2' Mo1' Co1' 125.45(15) . . ? C4' Mo1' Co1' 126.31(15) . . ? C3' Mo1' Co1' 111.88(15) . . ? Co2' Mo1' Co1' 54.20(2) . . ? C9' Co1' C11' 97.1(2) . . ? C9' Co1' C10' 103.4(3) . . ? C11' Co1' C10' 101.1(3) . . ? C9' Co1' C8' 102.8(2) . . ? C11' Co1' C8' 99.75(19) . . ? C10' Co1' C8' 143.9(2) . . ? C9' Co1' Co2' 150.54(17) . . ? C11' Co1' Co2' 94.36(14) . . ? C10' Co1' Co2' 100.81(19) . . ? C8' Co1' Co2' 48.38(15) . . ? C9' Co1' Mo1' 94.72(15) . . ? C11' Co1' Mo1' 147.40(16) . . ? C10' Co1' Mo1' 105.49(17) . . ? C8' Co1' Mo1' 47.88(12) . . ? Co2' Co1' Mo1' 62.55(2) . . ? C9 Co1 C11 98.7(2) . . ? C9 Co1 C10 102.3(3) . . ? C11 Co1 C10 102.2(2) . . ? C9 Co1 C8 106.0(2) . . ? C11 Co1 C8 95.5(2) . . ? C10 Co1 C8 143.8(2) . . ? C9 Co1 Co2 149.91(17) . . ? C11 Co1 Co2 99.26(14) . . ? C10 Co1 Co2 97.32(16) . . ? C8 Co1 Co2 48.29(13) . . ? C9 Co1 Mo1 88.44(15) . . ? C11 Co1 Mo1 143.79(18) . . ? C10 Co1 Mo1 110.91(16) . . ? C8 Co1 Mo1 48.75(12) . . ? Co2 Co1 Mo1 63.115(19) . . ? C12' Co2' C14' 98.7(2) . . ? C12' Co2' C13' 102.6(3) . . ? C14' Co2' C13' 103.0(3) . . ? C12' Co2' C8' 106.0(2) . . ? C14' Co2' C8' 96.4(2) . . ? C13' Co2' C8' 142.3(2) . . ? C12' Co2' Co1' 150.21(19) . . ? C14' Co2' Co1' 98.60(16) . . ? C13' Co2' Co1' 96.88(18) . . ? C8' Co2' Co1' 47.95(13) . . ? C12' Co2' Mo1' 88.93(17) . . ? C14' Co2' Mo1' 144.36(19) . . ? C13' Co2' Mo1' 109.22(17) . . ? C8' Co2' Mo1' 48.26(11) . . ? Co1' Co2' Mo1' 63.25(2) . . ? C12 Co2 C13 98.4(2) . . ? C12 Co2 C14 104.4(3) . . ? C13 Co2 C14 101.7(2) . . ? C12 Co2 C8 102.8(2) . . ? C13 Co2 C8 102.3(2) . . ? C14 Co2 C8 140.3(2) . . ? C12 Co2 Co1 150.31(18) . . ? C13 Co2 Co1 95.18(14) . . ? C14 Co2 Co1 98.53(19) . . ? C8 Co2 Co1 48.29(14) . . ? C12 Co2 Mo1 94.14(15) . . ? C13 Co2 Mo1 150.42(16) . . ? C14 Co2 Mo1 100.93(17) . . ? C8 Co2 Mo1 48.55(12) . . ? Co1 Co2 Mo1 62.75(2) . . ? C5 C1 C2 108.3(5) . . ? C5 C1 Mo1 72.8(3) . . ? C2 C1 Mo1 74.5(3) . . ? C5 C1 H1A 125.5 . . ? C2 C1 H1A 125.5 . . ? Mo1 C1 H1A 125.5 . . ? C2' C1' C5' 108.3(6) . . ? C2' C1' Mo1' 73.9(3) . . ? C5' C1' Mo1' 72.5(3) . . ? C2' C1' H1'A 125.6 . . ? C5' C1' H1'A 125.6 . . ? Mo1' C1' H1'A 125.6 . . ? C3 C2 C1 107.4(5) . . ? C3 C2 Mo1 72.4(3) . . ? C1 C2 Mo1 70.3(3) . . ? C3 C2 H2A 126.2 . . ? C1 C2 H2A 126.2 . . ? Mo1 C2 H2A 126.2 . . ? C1' C2' C3' 107.8(5) . . ? C1' C2' Mo1' 71.3(3) . . ? C3' C2' Mo1' 73.0(3) . . ? C1' C2' H2'A 126.0 . . ? C3' C2' H2'A 126.0 . . ? Mo1' C2' H2'A 126.0 . . ? C2 C3 C4 108.8(5) . . ? C2 C3 Mo1 72.9(4) . . ? C4 C3 Mo1 71.7(4) . . ? C2 C3 H3A 125.5 . . ? C4 C3 H3A 125.5 . . ? Mo1 C3 H3A 125.5 . . ? C4' C3' C2' 107.8(6) . . ? C4' C3' Mo1' 72.4(4) . . ? C2' C3' Mo1' 71.9(4) . . ? C4' C3' H3'A 125.9 . . ? C2' C3' H3'A 125.9 . . ? Mo1' C3' H3'A 125.9 . . ? C5' C4' C3' 107.9(5) . . ? C5' C4' Mo1' 71.3(3) . . ? C3' C4' Mo1' 72.8(4) . . ? C5' C4' H4'A 125.9 . . ? C3' C4' H4'A 125.9 . . ? Mo1' C4' H4'A 125.9 . . ? C3 C4 C5 107.4(5) . . ? C3 C4 Mo1 73.4(3) . . ? C5 C4 Mo1 71.7(3) . . ? C3 C4 H4A 126.1 . . ? C5 C4 H4A 126.1 . . ? Mo1 C4 H4A 126.1 . . ? C1 C5 C4 108.0(5) . . ? C1 C5 Mo1 71.9(2) . . ? C4 C5 Mo1 72.8(3) . . ? C1 C5 H5A 125.9 . . ? C4 C5 H5A 125.9 . . ? Mo1 C5 H5A 125.9 . . ? C4' C5' C1' 108.1(5) . . ? C4' C5' Mo1' 73.9(3) . . ? C1' C5' Mo1' 71.9(3) . . ? C4' C5' H5'A 125.7 . . ? C1' C5' H5'A 125.7 . . ? Mo1' C5' H5'A 125.7 . . ? O6 C6 Mo1 173.9(5) . . ? O6' C6' Mo1' 173.4(6) . . ? O7' C7' Mo1' 173.2(5) . . ? O7 C7 Mo1 171.7(5) . . ? F1' C8' Co1' 126.6(3) . . ? F1' C8' Co2' 125.6(3) . . ? Co1' C8' Co2' 83.7(2) . . ? F1' C8' Mo1' 129.3(3) . . ? Co1' C8' Mo1' 89.38(17) . . ? Co2' C8' Mo1' 88.33(19) . . ? F1 C8 Co1 126.4(3) . . ? F1 C8 Co2 127.5(3) . . ? Co1 C8 Co2 83.4(2) . . ? F1 C8 Mo1 128.8(3) . . ? Co1 C8 Mo1 88.04(19) . . ? Co2 C8 Mo1 88.41(17) . . ? O9' C9' Co1' 179.5(6) . . ? O9 C9 Co1 177.9(6) . . ? O10 C10 Co1 178.6(6) . . ? O10' C10' Co1' 178.8(7) . . ? O11 C11 Co1 178.2(5) . . ? O11' C11' Co1' 178.4(5) . . ? O12 C12 Co2 179.2(5) . . ? O12' C12' Co2' 178.4(6) . . ? O13 C13 Co2 178.8(5) . . ? O13' C13' Co2' 177.6(5) . . ? O14' C14' Co2' 178.0(6) . . ? O14 C14 Co2 177.2(7) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.762 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.089 #===END data_rph380 _database_code_depnum_ccdc_archive 'CCDC 793586' #TrackingRef '- allRPH.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H15 Co2 Cr F O8' _chemical_formula_weight 560.17 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 8.6778(5) _cell_length_b 11.1284(7) _cell_length_c 21.9659(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.2600(10) _cell_angle_gamma 90.00 _cell_volume 2112.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 6426 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.12 _exptl_crystal_description blade _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 2.109 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4858 _exptl_absorpt_correction_T_max 0.9019 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 17649 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0220 _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 -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.19 _reflns_number_total 4905 _reflns_number_gt 4584 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0300P)^2^+1.0000P] 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 4905 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0256 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0621 _refine_ls_wR_factor_gt 0.0610 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 Cr1 Cr 0.24533(3) 0.68813(2) 0.347608(11) 0.01155(7) Uani 1 1 d . . . Co1 Co 0.41388(2) 0.743764(18) 0.451215(9) 0.01299(6) Uani 1 1 d . . . Co2 Co 0.16087(2) 0.850037(19) 0.427101(10) 0.01562(6) Uani 1 1 d . . . F9 F 0.13999(11) 0.60575(9) 0.46937(4) 0.0194(2) Uani 1 1 d . . . O1 O 0.57200(14) 0.73189(11) 0.31971(5) 0.0209(2) Uani 1 1 d . . . O2 O 0.20557(15) 0.92193(11) 0.28021(6) 0.0241(3) Uani 1 1 d . . . O3 O 0.61927(15) 0.95332(12) 0.43677(6) 0.0293(3) Uani 1 1 d . . . O4 O 0.39798(16) 0.74514(12) 0.58424(6) 0.0275(3) Uani 1 1 d . . . O5 O 0.61334(14) 0.53221(11) 0.44640(6) 0.0238(3) Uani 1 1 d . . . O6 O -0.13998(15) 0.87625(13) 0.35647(7) 0.0329(3) Uani 1 1 d . . . O7 O 0.05616(18) 0.85974(14) 0.55064(6) 0.0374(4) Uani 1 1 d . . . O8 O 0.29515(16) 1.09046(12) 0.40878(7) 0.0337(3) Uani 1 1 d . . . C1 C 0.45063(18) 0.71797(14) 0.33679(7) 0.0155(3) Uani 1 1 d . . . C2 C 0.21816(18) 0.83733(15) 0.31092(7) 0.0170(3) Uani 1 1 d . . . C3 C 0.54202(19) 0.87182(15) 0.44033(7) 0.0187(3) Uani 1 1 d . . . C4 C 0.40434(19) 0.74700(14) 0.53306(8) 0.0188(3) Uani 1 1 d . . . C5 C 0.53704(18) 0.61476(15) 0.44851(7) 0.0167(3) Uani 1 1 d . . . C6 C -0.0239(2) 0.86449(15) 0.38427(8) 0.0220(3) Uani 1 1 d . . . C7 C 0.0983(2) 0.85810(16) 0.50349(9) 0.0246(4) Uani 1 1 d . . . C8 C 0.2433(2) 0.99819(16) 0.41485(8) 0.0227(4) Uani 1 1 d . . . C9 C 0.20960(18) 0.68411(14) 0.43330(7) 0.0140(3) Uani 1 1 d . . . C11 C 0.18684(18) 0.49178(14) 0.34444(7) 0.0149(3) Uani 1 1 d . . . C12 C 0.29144(18) 0.51816(14) 0.30016(7) 0.0164(3) Uani 1 1 d . . . C13 C 0.21766(19) 0.60300(14) 0.25796(7) 0.0177(3) Uani 1 1 d . . . C14 C 0.06679(19) 0.62710(14) 0.27583(7) 0.0171(3) Uani 1 1 d . . . C15 C 0.04786(18) 0.55865(14) 0.32933(7) 0.0156(3) Uani 1 1 d . . . C16 C 0.2126(2) 0.39752(14) 0.39309(8) 0.0199(3) Uani 1 1 d . . . H16A H 0.1734 0.3210 0.3772 0.030 Uiso 1 1 calc R . . H16B H 0.1586 0.4200 0.4281 0.030 Uiso 1 1 calc R . . H16C H 0.3225 0.3905 0.4054 0.030 Uiso 1 1 calc R . . C17 C 0.4421(2) 0.45565(16) 0.29421(8) 0.0236(4) Uani 1 1 d . . . H17A H 0.4232 0.3806 0.2723 0.035 Uiso 1 1 calc R . . H17B H 0.4927 0.4393 0.3346 0.035 Uiso 1 1 calc R . . H17C H 0.5081 0.5066 0.2719 0.035 Uiso 1 1 calc R . . C18 C 0.2821(2) 0.64944(17) 0.20133(8) 0.0258(4) Uani 1 1 d . . . H18A H 0.2543 0.5951 0.1676 0.039 Uiso 1 1 calc R . . H18B H 0.3939 0.6547 0.2083 0.039 Uiso 1 1 calc R . . H18C H 0.2398 0.7285 0.1916 0.039 Uiso 1 1 calc R . . C19 C -0.0565(2) 0.69851(16) 0.23969(8) 0.0250(4) Uani 1 1 d . . . H19A H -0.1184 0.6454 0.2123 0.038 Uiso 1 1 calc R . . H19B H -0.0086 0.7594 0.2161 0.038 Uiso 1 1 calc R . . H19C H -0.1222 0.7369 0.2674 0.038 Uiso 1 1 calc R . . C20 C -0.09878(19) 0.54719(16) 0.36040(8) 0.0216(3) Uani 1 1 d . . . H20A H -0.1590 0.4801 0.3429 0.032 Uiso 1 1 calc R . . H20B H -0.1586 0.6206 0.3546 0.032 Uiso 1 1 calc R . . H20C H -0.0734 0.5335 0.4038 0.032 Uiso 1 1 calc R . . 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 Cr1 0.01274(12) 0.01107(12) 0.01070(12) 0.00020(9) 0.00029(9) -0.00021(9) Co1 0.01395(11) 0.01271(11) 0.01208(11) -0.00082(7) -0.00012(8) 0.00061(7) Co2 0.01523(11) 0.01309(11) 0.01845(12) -0.00251(8) 0.00095(8) 0.00285(8) F9 0.0231(5) 0.0192(5) 0.0165(5) 0.0014(4) 0.0053(4) -0.0056(4) O1 0.0180(6) 0.0267(6) 0.0185(6) 0.0009(5) 0.0041(5) -0.0022(5) O2 0.0326(7) 0.0174(6) 0.0221(6) 0.0054(5) 0.0014(5) 0.0012(5) O3 0.0294(7) 0.0247(7) 0.0343(7) -0.0052(6) 0.0063(6) -0.0092(6) O4 0.0360(8) 0.0302(7) 0.0163(6) -0.0023(5) 0.0032(5) 0.0070(6) O5 0.0260(6) 0.0229(6) 0.0231(6) 0.0036(5) 0.0051(5) 0.0077(5) O6 0.0201(7) 0.0334(7) 0.0437(8) -0.0057(6) -0.0051(6) 0.0049(5) O7 0.0405(8) 0.0472(9) 0.0259(7) -0.0039(6) 0.0108(6) 0.0171(7) O8 0.0349(7) 0.0168(6) 0.0473(9) 0.0020(6) -0.0072(6) -0.0015(5) C1 0.0189(8) 0.0146(7) 0.0124(7) 0.0004(6) -0.0013(6) 0.0005(6) C2 0.0161(7) 0.0180(8) 0.0165(8) -0.0020(6) -0.0003(6) -0.0004(6) C3 0.0191(8) 0.0193(8) 0.0176(8) -0.0031(6) 0.0015(6) 0.0007(6) C4 0.0193(8) 0.0170(8) 0.0198(9) -0.0025(6) -0.0005(6) 0.0034(6) C5 0.0186(8) 0.0196(8) 0.0117(7) 0.0017(6) 0.0008(6) -0.0010(6) C6 0.0209(8) 0.0184(8) 0.0272(9) -0.0033(7) 0.0047(7) 0.0028(6) C7 0.0241(9) 0.0231(9) 0.0265(9) -0.0044(7) 0.0026(7) 0.0089(7) C8 0.0216(8) 0.0195(8) 0.0258(9) -0.0021(7) -0.0040(7) 0.0050(7) C9 0.0146(7) 0.0133(7) 0.0140(7) -0.0003(6) 0.0010(5) 0.0000(6) C11 0.0178(7) 0.0125(7) 0.0138(7) -0.0020(6) -0.0011(6) -0.0017(6) C12 0.0194(8) 0.0154(7) 0.0142(7) -0.0052(6) 0.0006(6) -0.0008(6) C13 0.0248(8) 0.0163(7) 0.0119(7) -0.0026(6) 0.0002(6) -0.0049(6) C14 0.0203(8) 0.0145(7) 0.0152(7) -0.0010(6) -0.0047(6) -0.0029(6) C15 0.0162(7) 0.0129(7) 0.0172(7) -0.0015(6) -0.0011(6) -0.0031(6) C16 0.0271(8) 0.0132(7) 0.0187(8) 0.0014(6) -0.0009(6) -0.0001(6) C17 0.0229(8) 0.0220(8) 0.0266(9) -0.0077(7) 0.0056(7) 0.0033(7) C18 0.0369(10) 0.0271(9) 0.0138(8) -0.0012(7) 0.0050(7) -0.0078(8) C19 0.0274(9) 0.0214(8) 0.0238(9) 0.0043(7) -0.0110(7) -0.0009(7) C20 0.0168(8) 0.0226(8) 0.0253(9) -0.0010(7) 0.0017(6) -0.0044(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 Cr1 C1 1.8489(16) . ? Cr1 C2 1.8512(17) . ? Cr1 C9 1.9360(16) . ? Cr1 C13 2.1786(15) . ? Cr1 C14 2.2136(15) . ? Cr1 C12 2.2137(15) . ? Cr1 C11 2.2429(15) . ? Cr1 C15 2.2467(15) . ? Cr1 Co2 2.6584(3) . ? Cr1 Co1 2.6630(3) . ? Co1 C5 1.7940(17) . ? Co1 C4 1.8077(17) . ? Co1 C3 1.8367(17) . ? Co1 C9 1.9000(16) . ? Co1 Co2 2.5073(3) . ? Co2 C6 1.7901(18) . ? Co2 C7 1.8125(19) . ? Co2 C8 1.8268(18) . ? Co2 C9 1.8964(15) . ? F9 C9 1.3569(18) . ? O1 C1 1.160(2) . ? O2 C2 1.158(2) . ? O3 C3 1.135(2) . ? O4 C4 1.131(2) . ? O5 C5 1.136(2) . ? O6 C6 1.137(2) . ? O7 C7 1.130(2) . ? O8 C8 1.134(2) . ? C11 C12 1.421(2) . ? C11 C15 1.430(2) . ? C11 C16 1.499(2) . ? C12 C13 1.432(2) . ? C12 C17 1.497(2) . ? C13 C14 1.426(2) . ? C13 C18 1.502(2) . ? C14 C15 1.423(2) . ? C14 C19 1.500(2) . ? C15 C20 1.504(2) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? 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 C1 Cr1 C2 82.46(7) . . ? C1 Cr1 C9 111.79(7) . . ? C2 Cr1 C9 114.75(7) . . ? C1 Cr1 C13 89.40(7) . . ? C2 Cr1 C13 89.85(7) . . ? C9 Cr1 C13 148.71(6) . . ? C1 Cr1 C14 125.69(7) . . ? C2 Cr1 C14 84.96(6) . . ? C9 Cr1 C14 121.43(6) . . ? C13 Cr1 C14 37.89(6) . . ? C1 Cr1 C12 82.82(6) . . ? C2 Cr1 C12 125.64(7) . . ? C9 Cr1 C12 119.33(6) . . ? C13 Cr1 C12 38.06(6) . . ? C14 Cr1 C12 63.09(6) . . ? C1 Cr1 C11 112.89(6) . . ? C2 Cr1 C11 147.23(6) . . ? C9 Cr1 C11 87.23(6) . . ? C13 Cr1 C11 62.77(6) . . ? C14 Cr1 C11 62.44(6) . . ? C12 Cr1 C11 37.17(6) . . ? C1 Cr1 C15 145.12(6) . . ? C2 Cr1 C15 115.64(6) . . ? C9 Cr1 C15 88.36(6) . . ? C13 Cr1 C15 62.65(6) . . ? C14 Cr1 C15 37.19(6) . . ? C12 Cr1 C15 62.33(6) . . ? C11 Cr1 C15 37.15(6) . . ? C1 Cr1 Co2 106.84(5) . . ? C2 Cr1 Co2 69.29(5) . . ? C9 Cr1 Co2 45.47(5) . . ? C13 Cr1 Co2 150.96(5) . . ? C14 Cr1 Co2 117.30(4) . . ? C12 Cr1 Co2 163.94(4) . . ? C11 Cr1 Co2 127.26(4) . . ? C15 Cr1 Co2 107.48(4) . . ? C1 Cr1 Co1 66.91(5) . . ? C2 Cr1 Co1 101.63(5) . . ? C9 Cr1 Co1 45.48(5) . . ? C13 Cr1 Co1 151.64(5) . . ? C14 Cr1 Co1 166.85(4) . . ? C12 Cr1 Co1 119.48(4) . . ? C11 Cr1 Co1 110.98(4) . . ? C15 Cr1 Co1 130.69(4) . . ? Co2 Cr1 Co1 56.220(8) . . ? C5 Co1 C4 97.50(7) . . ? C5 Co1 C3 104.30(7) . . ? C4 Co1 C3 101.39(7) . . ? C5 Co1 C9 105.12(7) . . ? C4 Co1 C9 94.94(7) . . ? C3 Co1 C9 143.97(7) . . ? C5 Co1 Co2 152.04(5) . . ? C4 Co1 Co2 94.68(5) . . ? C3 Co1 Co2 97.78(5) . . ? C9 Co1 Co2 48.61(5) . . ? C5 Co1 Cr1 93.89(5) . . ? C4 Co1 Cr1 141.53(6) . . ? C3 Co1 Cr1 111.15(5) . . ? C9 Co1 Cr1 46.59(5) . . ? Co2 Co1 Cr1 61.796(9) . . ? C6 Co2 C7 98.76(8) . . ? C6 Co2 C8 100.68(8) . . ? C7 Co2 C8 104.25(8) . . ? C6 Co2 C9 107.96(7) . . ? C7 Co2 C9 93.76(7) . . ? C8 Co2 C9 143.28(7) . . ? C6 Co2 Co1 151.41(5) . . ? C7 Co2 Co1 99.12(6) . . ? C8 Co2 Co1 96.30(5) . . ? C9 Co2 Co1 48.73(5) . . ? C6 Co2 Cr1 90.18(5) . . ? C7 Co2 Cr1 139.96(6) . . ? C8 Co2 Cr1 112.31(6) . . ? C9 Co2 Cr1 46.70(5) . . ? Co1 Co2 Cr1 61.983(9) . . ? O1 C1 Cr1 168.35(14) . . ? O2 C2 Cr1 169.95(14) . . ? O3 C3 Co1 176.09(15) . . ? O4 C4 Co1 177.80(15) . . ? O5 C5 Co1 179.04(16) . . ? O6 C6 Co2 178.31(17) . . ? O7 C7 Co2 177.61(18) . . ? O8 C8 Co2 178.30(17) . . ? F9 C9 Co2 124.01(11) . . ? F9 C9 Co1 124.09(11) . . ? Co2 C9 Co1 82.67(6) . . ? F9 C9 Cr1 134.61(11) . . ? Co2 C9 Cr1 87.83(6) . . ? Co1 C9 Cr1 87.93(6) . . ? C12 C11 C15 108.16(13) . . ? C12 C11 C16 124.73(14) . . ? C15 C11 C16 126.65(14) . . ? C12 C11 Cr1 70.30(9) . . ? C15 C11 Cr1 71.57(9) . . ? C16 C11 Cr1 129.86(11) . . ? C11 C12 C13 107.67(14) . . ? C11 C12 C17 125.57(15) . . ? C13 C12 C17 126.28(15) . . ? C11 C12 Cr1 72.53(9) . . ? C13 C12 Cr1 69.64(9) . . ? C17 C12 Cr1 129.42(11) . . ? C14 C13 C12 108.23(14) . . ? C14 C13 C18 125.75(15) . . ? C12 C13 C18 125.78(16) . . ? C14 C13 Cr1 72.38(9) . . ? C12 C13 Cr1 72.30(9) . . ? C18 C13 Cr1 125.49(11) . . ? C15 C14 C13 107.76(14) . . ? C15 C14 C19 126.17(15) . . ? C13 C14 C19 125.59(15) . . ? C15 C14 Cr1 72.67(9) . . ? C13 C14 Cr1 69.73(9) . . ? C19 C14 Cr1 129.27(12) . . ? C14 C15 C11 108.16(14) . . ? C14 C15 C20 125.95(14) . . ? C11 C15 C20 125.54(14) . . ? C14 C15 Cr1 70.14(9) . . ? C11 C15 Cr1 71.28(9) . . ? C20 C15 Cr1 129.55(11) . . ? 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 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.399 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.068 #===END data_rph386 _database_code_depnum_ccdc_archive 'CCDC 793587' #TrackingRef '- allRPH.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H15 Co2 F O8 W' _chemical_formula_weight 692.02 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 8.859(2) _cell_length_b 11.199(3) _cell_length_c 22.190(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.370(5) _cell_angle_gamma 90.00 _cell_volume 2197.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 5084 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 28.15 _exptl_crystal_description block _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.092 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 6.764 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2361 _exptl_absorpt_correction_T_max 0.5511 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 15475 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0385 _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 -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.17 _reflns_number_total 5135 _reflns_number_gt 4679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0300P)^2^+2.0000P] 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 5135 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0668 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 W1 W 0.253004(16) 0.685408(13) 0.348357(6) 0.02380(6) Uani 1 1 d . . . Co1 Co 0.41237(6) 0.74389(5) 0.45460(2) 0.02733(12) Uani 1 1 d . . . Co2 Co 0.16524(6) 0.84787(5) 0.43220(3) 0.03332(14) Uani 1 1 d . . . F9 F 0.1433(3) 0.6041(2) 0.47346(11) 0.0416(6) Uani 1 1 d . . . O1 O 0.5902(4) 0.7215(3) 0.32030(15) 0.0482(8) Uani 1 1 d . . . O2 O 0.2065(4) 0.9265(3) 0.27996(16) 0.0567(10) Uani 1 1 d . . . O3 O 0.6115(5) 0.9505(4) 0.4336(2) 0.0679(11) Uani 1 1 d . . . O4 O 0.3959(5) 0.7447(4) 0.58571(15) 0.0647(11) Uani 1 1 d . . . O5 O 0.6097(4) 0.5367(3) 0.44573(15) 0.0530(9) Uani 1 1 d . . . O6 O -0.1251(4) 0.8674(4) 0.3642(2) 0.0753(13) Uani 1 1 d . . . O7 O 0.0638(5) 0.8618(5) 0.55538(19) 0.0792(14) Uani 1 1 d . . . O8 O 0.2917(5) 1.0854(3) 0.4081(2) 0.0783(14) Uani 1 1 d . . . C1 C 0.4678(5) 0.7134(4) 0.33529(19) 0.0337(9) Uani 1 1 d . . . C2 C 0.2256(5) 0.8415(4) 0.3093(2) 0.0356(9) Uani 1 1 d . . . C3 C 0.5356(5) 0.8700(4) 0.4404(2) 0.0407(10) Uani 1 1 d . . . C4 C 0.4019(5) 0.7471(4) 0.5351(2) 0.0388(10) Uani 1 1 d . . . C5 C 0.5344(5) 0.6174(4) 0.44965(19) 0.0352(9) Uani 1 1 d . . . C6 C -0.0123(5) 0.8589(5) 0.3914(2) 0.0476(12) Uani 1 1 d . . . C7 C 0.1040(6) 0.8583(5) 0.5079(3) 0.0529(13) Uani 1 1 d . . . C8 C 0.2428(6) 0.9945(5) 0.4165(2) 0.0508(13) Uani 1 1 d . . . C9 C 0.2139(5) 0.6834(3) 0.43794(19) 0.0287(8) Uani 1 1 d . . . C11 C 0.1840(5) 0.4809(4) 0.34417(18) 0.0317(9) Uani 1 1 d . . . C12 C 0.2890(5) 0.5052(4) 0.2992(2) 0.0376(10) Uani 1 1 d . . . C13 C 0.2209(5) 0.5879(4) 0.25745(18) 0.0377(10) Uani 1 1 d . . . C14 C 0.0738(5) 0.6158(4) 0.27638(19) 0.0350(9) Uani 1 1 d . . . C15 C 0.0513(4) 0.5488(4) 0.32978(18) 0.0320(9) Uani 1 1 d . . . C16 C 0.2047(6) 0.3889(4) 0.3927(2) 0.0435(11) Uani 1 1 d . . . H16A H 0.1665 0.3127 0.3776 0.065 Uiso 1 1 calc R . . H16B H 0.1496 0.4128 0.4272 0.065 Uiso 1 1 calc R . . H16C H 0.3113 0.3815 0.4047 0.065 Uiso 1 1 calc R . . C17 C 0.4365(6) 0.4413(5) 0.2932(3) 0.0573(14) Uani 1 1 d . . . H17A H 0.4184 0.3669 0.2715 0.086 Uiso 1 1 calc R . . H17B H 0.4827 0.4245 0.3330 0.086 Uiso 1 1 calc R . . H17C H 0.5037 0.4912 0.2711 0.086 Uiso 1 1 calc R . . C18 C 0.2858(7) 0.6301(6) 0.2000(2) 0.0628(16) Uani 1 1 d . . . H18A H 0.2569 0.5752 0.1675 0.094 Uiso 1 1 calc R . . H18B H 0.3952 0.6332 0.2054 0.094 Uiso 1 1 calc R . . H18C H 0.2471 0.7091 0.1899 0.094 Uiso 1 1 calc R . . C19 C -0.0445(6) 0.6885(4) 0.2413(3) 0.0541(14) Uani 1 1 d . . . H19A H -0.1049 0.6365 0.2145 0.081 Uiso 1 1 calc R . . H19B H 0.0045 0.7485 0.2177 0.081 Uiso 1 1 calc R . . H19C H -0.1093 0.7273 0.2691 0.081 Uiso 1 1 calc R . . C20 C -0.0926(5) 0.5398(5) 0.3616(2) 0.0459(12) Uani 1 1 d . . . H20A H -0.1528 0.4741 0.3448 0.069 Uiso 1 1 calc R . . H20B H -0.1490 0.6137 0.3564 0.069 Uiso 1 1 calc R . . H20C H -0.0693 0.5257 0.4043 0.069 Uiso 1 1 calc R . . 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 W1 0.02519(9) 0.02373(9) 0.02229(9) 0.00084(6) -0.00013(6) -0.00006(6) Co1 0.0284(3) 0.0285(3) 0.0248(3) -0.0023(2) -0.0010(2) 0.0027(2) Co2 0.0305(3) 0.0282(3) 0.0412(3) -0.0066(2) 0.0013(2) 0.0066(2) F9 0.0534(15) 0.0414(15) 0.0314(13) 0.0000(11) 0.0143(11) -0.0141(12) O1 0.0317(17) 0.072(2) 0.0420(19) 0.0059(17) 0.0107(14) -0.0010(16) O2 0.078(3) 0.041(2) 0.051(2) 0.0197(17) 0.0024(19) 0.0099(18) O3 0.063(2) 0.053(2) 0.089(3) -0.009(2) 0.019(2) -0.022(2) O4 0.088(3) 0.074(3) 0.0324(19) -0.0062(18) 0.0052(19) 0.027(2) O5 0.057(2) 0.053(2) 0.050(2) 0.0110(17) 0.0144(17) 0.0255(18) O6 0.041(2) 0.077(3) 0.104(3) -0.024(3) -0.018(2) 0.019(2) O7 0.080(3) 0.103(4) 0.056(3) -0.019(2) 0.020(2) 0.034(3) O8 0.082(3) 0.031(2) 0.120(4) 0.007(2) -0.015(3) -0.006(2) C1 0.034(2) 0.039(2) 0.028(2) 0.0063(18) -0.0018(17) 0.0005(18) C2 0.038(2) 0.034(2) 0.035(2) 0.0042(19) -0.0012(18) 0.0025(18) C3 0.040(2) 0.040(3) 0.042(3) -0.008(2) 0.007(2) 0.000(2) C4 0.043(2) 0.039(3) 0.034(2) -0.003(2) 0.0018(19) 0.009(2) C5 0.038(2) 0.039(2) 0.029(2) 0.0072(18) 0.0051(17) 0.0064(19) C6 0.037(3) 0.042(3) 0.064(3) -0.011(2) 0.001(2) 0.010(2) C7 0.053(3) 0.050(3) 0.057(3) -0.017(3) 0.006(3) 0.017(2) C8 0.050(3) 0.038(3) 0.062(3) -0.007(2) -0.015(2) 0.014(2) C9 0.030(2) 0.024(2) 0.032(2) -0.0016(16) 0.0030(16) -0.0018(15) C11 0.043(2) 0.023(2) 0.028(2) -0.0031(16) -0.0006(17) -0.0042(17) C12 0.046(3) 0.030(2) 0.037(2) -0.0134(18) 0.0036(19) -0.0003(19) C13 0.051(3) 0.040(2) 0.0223(19) -0.0054(17) -0.0001(18) -0.014(2) C14 0.042(2) 0.028(2) 0.034(2) 0.0029(17) -0.0127(18) -0.0078(18) C15 0.030(2) 0.032(2) 0.034(2) -0.0022(17) -0.0029(17) -0.0077(17) C16 0.062(3) 0.024(2) 0.044(3) 0.0022(19) -0.004(2) -0.003(2) C17 0.058(3) 0.048(3) 0.068(4) -0.020(3) 0.017(3) 0.014(2) C18 0.088(4) 0.075(4) 0.026(2) -0.006(3) 0.008(3) -0.032(3) C19 0.059(3) 0.048(3) 0.052(3) 0.014(2) -0.028(3) -0.009(2) C20 0.030(2) 0.052(3) 0.056(3) 0.000(2) 0.002(2) -0.008(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 W1 C2 1.960(4) . ? W1 C1 1.967(4) . ? W1 C9 2.038(4) . ? W1 C13 2.297(4) . ? W1 C14 2.320(4) . ? W1 C12 2.325(4) . ? W1 C15 2.370(4) . ? W1 C11 2.371(4) . ? W1 Co2 2.7471(7) . ? W1 Co1 2.7547(8) . ? Co1 C5 1.789(4) . ? Co1 C4 1.794(4) . ? Co1 C3 1.824(5) . ? Co1 C9 1.900(4) . ? Co1 Co2 2.5035(9) . ? Co2 C6 1.772(5) . ? Co2 C7 1.800(6) . ? Co2 C8 1.821(6) . ? Co2 C9 1.894(4) . ? F9 C9 1.364(4) . ? O1 C1 1.157(5) . ? O2 C2 1.160(5) . ? O3 C3 1.140(6) . ? O4 C4 1.128(5) . ? O5 C5 1.129(5) . ? O6 C6 1.141(6) . ? O7 C7 1.132(6) . ? O8 C8 1.127(6) . ? C11 C15 1.420(6) . ? C11 C12 1.430(6) . ? C11 C16 1.493(6) . ? C12 C13 1.419(6) . ? C12 C17 1.503(6) . ? C13 C14 1.427(6) . ? C13 C18 1.506(6) . ? C14 C15 1.426(6) . ? C14 C19 1.508(6) . ? C15 C20 1.497(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? 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 W1 C1 83.60(18) . . ? C2 W1 C9 114.68(17) . . ? C1 W1 C9 111.52(17) . . ? C2 W1 C13 91.69(18) . . ? C1 W1 C13 90.99(17) . . ? C9 W1 C13 146.34(15) . . ? C2 W1 C14 86.17(17) . . ? C1 W1 C14 125.52(17) . . ? C9 W1 C14 121.29(16) . . ? C13 W1 C14 36.00(16) . . ? C2 W1 C12 125.68(18) . . ? C1 W1 C12 84.76(17) . . ? C9 W1 C12 118.96(16) . . ? C13 W1 C12 35.76(16) . . ? C14 W1 C12 59.48(16) . . ? C2 W1 C15 115.23(17) . . ? C1 W1 C15 143.44(17) . . ? C9 W1 C15 89.61(15) . . ? C13 W1 C15 59.14(15) . . ? C14 W1 C15 35.39(14) . . ? C12 W1 C15 58.71(15) . . ? C2 W1 C11 145.00(17) . . ? C1 W1 C11 113.42(17) . . ? C9 W1 C11 88.26(14) . . ? C13 W1 C11 59.20(14) . . ? C14 W1 C11 58.92(14) . . ? C12 W1 C11 35.43(14) . . ? C15 W1 C11 34.87(14) . . ? C2 W1 Co2 71.12(13) . . ? C1 W1 Co2 108.00(13) . . ? C9 W1 Co2 43.57(11) . . ? C13 W1 Co2 152.17(12) . . ? C14 W1 Co2 118.66(12) . . ? C12 W1 Co2 160.87(11) . . ? C15 W1 Co2 107.76(10) . . ? C11 W1 Co2 125.72(10) . . ? C2 W1 Co1 102.16(13) . . ? C1 W1 Co1 68.70(12) . . ? C9 W1 Co1 43.58(12) . . ? C13 W1 Co1 153.58(12) . . ? C14 W1 Co1 164.73(11) . . ? C12 W1 Co1 122.04(12) . . ? C15 W1 Co1 130.20(10) . . ? C11 W1 Co1 112.40(10) . . ? Co2 W1 Co1 54.13(2) . . ? C5 Co1 C4 98.27(19) . . ? C5 Co1 C3 103.5(2) . . ? C4 Co1 C3 102.9(2) . . ? C5 Co1 C9 105.17(19) . . ? C4 Co1 C9 95.7(2) . . ? C3 Co1 C9 143.0(2) . . ? C5 Co1 Co2 151.71(15) . . ? C4 Co1 Co2 95.31(15) . . ? C3 Co1 Co2 97.50(15) . . ? C9 Co1 Co2 48.61(12) . . ? C5 Co1 W1 92.31(14) . . ? C4 Co1 W1 143.41(16) . . ? C3 Co1 W1 108.55(15) . . ? C9 Co1 W1 47.70(12) . . ? Co2 Co1 W1 62.78(2) . . ? C6 Co2 C7 99.5(2) . . ? C6 Co2 C8 100.0(2) . . ? C7 Co2 C8 104.9(3) . . ? C6 Co2 C9 107.1(2) . . ? C7 Co2 C9 94.6(2) . . ? C8 Co2 C9 143.4(2) . . ? C6 Co2 Co1 150.83(16) . . ? C7 Co2 Co1 98.80(17) . . ? C8 Co2 Co1 97.00(16) . . ? C9 Co2 Co1 48.80(13) . . ? C6 Co2 W1 88.75(16) . . ? C7 Co2 W1 142.02(18) . . ? C8 Co2 W1 110.04(17) . . ? C9 Co2 W1 47.87(13) . . ? Co1 Co2 W1 63.09(2) . . ? O1 C1 W1 170.7(4) . . ? O2 C2 W1 172.1(4) . . ? O3 C3 Co1 177.4(4) . . ? O4 C4 Co1 177.5(4) . . ? O5 C5 Co1 178.7(5) . . ? O6 C6 Co2 178.5(6) . . ? O7 C7 Co2 178.1(6) . . ? O8 C8 Co2 178.6(5) . . ? F9 C9 Co2 124.2(3) . . ? F9 C9 Co1 124.8(3) . . ? Co2 C9 Co1 82.59(15) . . ? F9 C9 W1 132.9(3) . . ? Co2 C9 W1 88.57(17) . . ? Co1 C9 W1 88.72(16) . . ? C15 C11 C12 107.7(4) . . ? C15 C11 C16 126.6(4) . . ? C12 C11 C16 125.3(4) . . ? C15 C11 W1 72.5(2) . . ? C12 C11 W1 70.5(2) . . ? C16 C11 W1 128.2(3) . . ? C13 C12 C11 108.1(4) . . ? C13 C12 C17 126.2(4) . . ? C11 C12 C17 125.2(4) . . ? C13 C12 W1 71.0(2) . . ? C11 C12 W1 74.0(2) . . ? C17 C12 W1 126.8(3) . . ? C12 C13 C14 108.1(4) . . ? C12 C13 C18 126.1(5) . . ? C14 C13 C18 125.6(5) . . ? C12 C13 W1 73.2(2) . . ? C14 C13 W1 72.9(2) . . ? C18 C13 W1 124.1(3) . . ? C15 C14 C13 107.7(4) . . ? C15 C14 C19 125.9(4) . . ? C13 C14 C19 125.8(4) . . ? C15 C14 W1 74.2(2) . . ? C13 C14 W1 71.1(2) . . ? C19 C14 W1 126.9(3) . . ? C11 C15 C14 108.3(4) . . ? C11 C15 C20 125.1(4) . . ? C14 C15 C20 126.3(4) . . ? C11 C15 W1 72.6(2) . . ? C14 C15 W1 70.4(2) . . ? C20 C15 W1 128.0(3) . . ? 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 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.334 _refine_diff_density_min -1.127 _refine_diff_density_rms 0.126 #===END data_rph352 _database_code_depnum_ccdc_archive 'CCDC 793588' #TrackingRef '- allRPH.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H33 F Mo O P2' _chemical_formula_weight 430.31 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' F F 0.0171 0.0103 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.616(2) _cell_length_b 9.1616(15) _cell_length_c 16.705(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.271(3) _cell_angle_gamma 90.00 _cell_volume 2078.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 6039 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.84 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7421 _exptl_absorpt_correction_T_max 0.9540 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 9646 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.11 _reflns_number_total 4115 _reflns_number_gt 3488 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0650P)^2^+0.1000P] 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 4115 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1103 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Mo1 Mo 0.745320(18) -0.04000(2) 0.179465(14) 0.02496(12) Uani 1 1 d . . . P1 P 0.87951(6) -0.21641(8) 0.19252(5) 0.0342(2) Uani 1 1 d . . . P2 P 0.69886(6) 0.07713(9) 0.30204(5) 0.0329(2) Uani 1 1 d . . . O2 O 0.6494(2) -0.2922(2) 0.26610(16) 0.0565(7) Uani 1 1 d . . . F1 F 0.87123(13) 0.07359(17) 0.22844(11) 0.0365(4) Uani 1 1 d . . . C1 C 0.7528(3) -0.0350(3) 0.0381(2) 0.0369(8) Uani 1 1 d . . . C2 C 0.7487(3) 0.1121(3) 0.06211(19) 0.0364(7) Uani 1 1 d . . . C3 C 0.6597(3) 0.1351(3) 0.09822(19) 0.0370(8) Uani 1 1 d . . . C4 C 0.6068(2) 0.0006(3) 0.0980(2) 0.0343(7) Uani 1 1 d . . . C5 C 0.6653(2) -0.1050(3) 0.06051(18) 0.0342(7) Uani 1 1 d . . . C6 C 0.8241(3) -0.0978(4) -0.0160(2) 0.0527(10) Uani 1 1 d . . . H6A H 0.8035 -0.0734 -0.0713 0.079 Uiso 1 1 calc R . . H6B H 0.8261 -0.2030 -0.0099 0.079 Uiso 1 1 calc R . . H6C H 0.8891 -0.0576 -0.0022 0.079 Uiso 1 1 calc R . . C7 C 0.8293(3) 0.2225(4) 0.0548(2) 0.0513(10) Uani 1 1 d . . . H7A H 0.8191 0.2729 0.0038 0.077 Uiso 1 1 calc R . . H7B H 0.8925 0.1732 0.0576 0.077 Uiso 1 1 calc R . . H7C H 0.8283 0.2925 0.0983 0.077 Uiso 1 1 calc R . . C8 C 0.6192(3) 0.2813(3) 0.1208(2) 0.0539(10) Uani 1 1 d . . . H8A H 0.5872 0.3274 0.0734 0.081 Uiso 1 1 calc R . . H8B H 0.6726 0.3429 0.1427 0.081 Uiso 1 1 calc R . . H8C H 0.5717 0.2678 0.1606 0.081 Uiso 1 1 calc R . . C9 C 0.5032(3) -0.0239(4) 0.1183(2) 0.0502(10) Uani 1 1 d . . . H9A H 0.4585 0.0012 0.0724 0.075 Uiso 1 1 calc R . . H9B H 0.4893 0.0368 0.1637 0.075 Uiso 1 1 calc R . . H9C H 0.4944 -0.1258 0.1319 0.075 Uiso 1 1 calc R . . C10 C 0.6318(3) -0.2560(4) 0.0358(2) 0.0475(9) Uani 1 1 d . . . H10A H 0.5989 -0.2526 -0.0177 0.071 Uiso 1 1 calc R . . H10B H 0.5865 -0.2924 0.0732 0.071 Uiso 1 1 calc R . . H10C H 0.6884 -0.3202 0.0358 0.071 Uiso 1 1 calc R . . C11 C 0.8569(3) -0.4027(3) 0.1585(3) 0.0641(12) Uani 1 1 d . . . H11A H 0.9168 -0.4594 0.1676 0.096 Uiso 1 1 calc R . . H11B H 0.8362 -0.4024 0.1017 0.096 Uiso 1 1 calc R . . H11C H 0.8055 -0.4457 0.1882 0.096 Uiso 1 1 calc R . . C12 C 0.9932(3) -0.1729(4) 0.1475(2) 0.0536(10) Uani 1 1 d . . . H12A H 1.0398 -0.2522 0.1572 0.080 Uiso 1 1 calc R . . H12B H 1.0209 -0.0839 0.1710 0.080 Uiso 1 1 calc R . . H12C H 0.9797 -0.1595 0.0901 0.080 Uiso 1 1 calc R . . C13 C 0.9263(3) -0.2444(4) 0.2951(2) 0.0512(9) Uani 1 1 d . . . H13A H 0.9793 -0.3154 0.2968 0.077 Uiso 1 1 calc R . . H13B H 0.8738 -0.2803 0.3260 0.077 Uiso 1 1 calc R . . H13C H 0.9510 -0.1528 0.3176 0.077 Uiso 1 1 calc R . . C14 C 0.5742(3) 0.0570(4) 0.3311(3) 0.0555(10) Uani 1 1 d . . . H14A H 0.5672 0.1095 0.3808 0.083 Uiso 1 1 calc R . . H14B H 0.5600 -0.0456 0.3388 0.083 Uiso 1 1 calc R . . H14C H 0.5284 0.0964 0.2893 0.083 Uiso 1 1 calc R . . C15 C 0.7693(3) 0.0037(4) 0.3895(2) 0.0524(10) Uani 1 1 d . . . H15A H 0.7496 0.0520 0.4374 0.079 Uiso 1 1 calc R . . H15B H 0.8389 0.0202 0.3844 0.079 Uiso 1 1 calc R . . H15C H 0.7570 -0.1002 0.3933 0.079 Uiso 1 1 calc R . . C16 C 0.7208(3) 0.2712(3) 0.3159(2) 0.0449(8) Uani 1 1 d . . . H16A H 0.6985 0.3014 0.3672 0.067 Uiso 1 1 calc R . . H16B H 0.6849 0.3249 0.2731 0.067 Uiso 1 1 calc R . . H16C H 0.7907 0.2910 0.3149 0.067 Uiso 1 1 calc R . . C17 C 0.6870(2) -0.1951(3) 0.23358(19) 0.0348(7) 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 Mo1 0.0226(2) 0.02372(14) 0.02858(18) -0.00095(9) 0.00180(13) -0.00099(8) P1 0.0287(5) 0.0283(4) 0.0458(5) -0.0004(3) 0.0037(4) 0.0030(3) P2 0.0316(5) 0.0353(4) 0.0320(5) -0.0045(3) 0.0039(4) -0.0001(3) O2 0.0563(18) 0.0475(13) 0.0671(18) 0.0107(12) 0.0132(14) -0.0185(12) F1 0.0284(11) 0.0338(8) 0.0468(11) -0.0049(8) 0.0004(9) -0.0076(7) C1 0.039(2) 0.0444(18) 0.0274(17) -0.0020(12) 0.0009(16) 0.0010(13) C2 0.040(2) 0.0376(15) 0.0302(17) 0.0067(13) -0.0052(15) -0.0052(14) C3 0.040(2) 0.0339(14) 0.0354(18) 0.0018(13) -0.0077(16) 0.0042(13) C4 0.028(2) 0.0392(14) 0.0339(18) -0.0041(13) -0.0075(15) 0.0001(13) C5 0.0336(19) 0.0373(15) 0.0309(17) -0.0061(12) -0.0038(15) -0.0046(13) C6 0.053(3) 0.070(2) 0.036(2) -0.0024(18) 0.0145(19) 0.0009(19) C7 0.057(3) 0.0460(18) 0.049(2) 0.0181(16) -0.0065(19) -0.0137(17) C8 0.064(3) 0.0400(17) 0.055(2) -0.0003(16) -0.014(2) 0.0173(17) C9 0.028(2) 0.066(2) 0.055(3) -0.0106(18) -0.0042(19) 0.0031(16) C10 0.047(2) 0.0454(17) 0.050(2) -0.0150(16) -0.0015(18) -0.0108(16) C11 0.061(3) 0.0276(16) 0.103(4) -0.0102(19) -0.005(2) 0.0055(16) C12 0.036(2) 0.061(2) 0.065(3) 0.0001(19) 0.015(2) 0.0052(17) C13 0.044(2) 0.057(2) 0.052(2) 0.0146(17) 0.0004(19) 0.0162(17) C14 0.047(3) 0.064(2) 0.059(3) -0.0135(19) 0.020(2) -0.0061(18) C15 0.066(3) 0.0511(18) 0.039(2) -0.0060(16) -0.004(2) 0.0026(19) C16 0.048(2) 0.0374(16) 0.049(2) -0.0081(14) -0.0001(17) 0.0023(15) C17 0.0314(19) 0.0346(15) 0.0386(18) -0.0012(13) 0.0028(15) -0.0021(12) _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 Mo1 C17 1.890(3) . ? Mo1 F1 2.1172(17) . ? Mo1 C4 2.273(3) . ? Mo1 C5 2.274(3) . ? Mo1 C3 2.354(3) . ? Mo1 C1 2.372(3) . ? Mo1 C2 2.409(3) . ? Mo1 P2 2.4367(9) . ? Mo1 P1 2.4369(9) . ? P1 C13 1.801(4) . ? P1 C12 1.815(4) . ? P1 C11 1.818(3) . ? P2 C14 1.810(4) . ? P2 C16 1.815(3) . ? P2 C15 1.815(4) . ? O2 C17 1.180(4) . ? C1 C2 1.409(4) . ? C1 C5 1.427(5) . ? C1 C6 1.490(5) . ? C2 C3 1.409(5) . ? C2 C7 1.504(4) . ? C3 C4 1.428(4) . ? C3 C8 1.507(4) . ? C4 C5 1.427(4) . ? C4 C9 1.492(5) . ? C5 C10 1.504(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? 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 C17 Mo1 F1 122.78(11) . . ? C17 Mo1 C4 92.87(13) . . ? F1 Mo1 C4 139.73(9) . . ? C17 Mo1 C5 91.72(12) . . ? F1 Mo1 C5 142.02(9) . . ? C4 Mo1 C5 36.59(11) . . ? C17 Mo1 C3 125.50(13) . . ? F1 Mo1 C3 103.88(9) . . ? C4 Mo1 C3 35.90(11) . . ? C5 Mo1 C3 59.33(11) . . ? C17 Mo1 C1 122.77(12) . . ? F1 Mo1 C1 106.38(10) . . ? C4 Mo1 C1 59.72(12) . . ? C5 Mo1 C1 35.71(11) . . ? C3 Mo1 C1 57.91(11) . . ? C17 Mo1 C2 149.14(12) . . ? F1 Mo1 C2 88.06(9) . . ? C4 Mo1 C2 58.89(12) . . ? C5 Mo1 C2 58.48(11) . . ? C3 Mo1 C2 34.39(11) . . ? C1 Mo1 C2 34.27(11) . . ? C17 Mo1 P2 77.56(9) . . ? F1 Mo1 P2 73.27(5) . . ? C4 Mo1 P2 100.09(9) . . ? C5 Mo1 P2 135.42(9) . . ? C3 Mo1 P2 92.06(8) . . ? C1 Mo1 P2 149.46(8) . . ? C2 Mo1 P2 116.81(8) . . ? C17 Mo1 P1 78.31(10) . . ? F1 Mo1 P1 73.22(5) . . ? C4 Mo1 P1 138.19(8) . . ? C5 Mo1 P1 102.24(8) . . ? C3 Mo1 P1 147.10(9) . . ? C1 Mo1 P1 90.83(8) . . ? C2 Mo1 P1 113.39(9) . . ? P2 Mo1 P1 117.18(3) . . ? C13 P1 C12 99.99(18) . . ? C13 P1 C11 101.71(19) . . ? C12 P1 C11 101.92(19) . . ? C13 P1 Mo1 112.92(12) . . ? C12 P1 Mo1 118.31(12) . . ? C11 P1 Mo1 119.10(13) . . ? C14 P2 C16 102.36(17) . . ? C14 P2 C15 101.3(2) . . ? C16 P2 C15 100.84(17) . . ? C14 P2 Mo1 119.22(13) . . ? C16 P2 Mo1 119.24(12) . . ? C15 P2 Mo1 110.99(13) . . ? C2 C1 C5 107.7(3) . . ? C2 C1 C6 125.7(3) . . ? C5 C1 C6 125.5(3) . . ? C2 C1 Mo1 74.30(18) . . ? C5 C1 Mo1 68.40(18) . . ? C6 C1 Mo1 132.4(2) . . ? C1 C2 C3 108.6(3) . . ? C1 C2 C7 125.1(3) . . ? C3 C2 C7 126.2(3) . . ? C1 C2 Mo1 71.43(18) . . ? C3 C2 Mo1 70.67(17) . . ? C7 C2 Mo1 120.9(2) . . ? C2 C3 C4 108.6(3) . . ? C2 C3 C8 125.6(3) . . ? C4 C3 C8 125.0(3) . . ? C2 C3 Mo1 74.94(18) . . ? C4 C3 Mo1 68.96(17) . . ? C8 C3 Mo1 129.5(2) . . ? C5 C4 C3 106.8(3) . . ? C5 C4 C9 124.4(3) . . ? C3 C4 C9 127.9(3) . . ? C5 C4 Mo1 71.75(19) . . ? C3 C4 Mo1 75.15(18) . . ? C9 C4 Mo1 126.6(2) . . ? C4 C5 C1 108.3(3) . . ? C4 C5 C10 125.2(3) . . ? C1 C5 C10 125.6(3) . . ? C4 C5 Mo1 71.66(18) . . ? C1 C5 Mo1 75.89(18) . . ? C10 C5 Mo1 126.6(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 . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P1 C12 H12A 109.5 . . ? P1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P2 C14 H14A 109.5 . . ? P2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? P2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? P2 C15 H15A 109.5 . . ? P2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P2 C16 H16A 109.5 . . ? P2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O2 C17 Mo1 178.7(3) . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.854 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.095 #===END