Homo- and Heteropolynuclear Complexes Containing Bidentate Bridging 4-Phosphino-N-Heterocyclic Carbene Ligands.
Han, Zeyu; Bates, Joshua I.; Strehl, Dominik; Patrick, Brian O.; Gates, Derek P.; Inorganic chemistry 55 (2016) 5071–5078; doi:10.1021/acs.inorgchem.6b00686

data_4347842
_publ_section_title
;
 Homo- and Heteropolynuclear Complexes Containing Bidentate Bridging
 4-Phosphino-N-Heterocyclic Carbene Ligands.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5071
_journal_page_last               5078
_journal_paper_doi               10.1021/acs.inorgchem.6b00686
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C47 H53 Au Cl3 N2 P Pd S, 2(C H2 Cl2)'
_chemical_formula_sum            'C49 H57 Au Cl7 N2 P Pd S'
_chemical_formula_weight         1288.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.275(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4990(15)
_cell_length_b                   20.5435(18)
_cell_length_c                   18.1531(17)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.14
_cell_measurement_theta_min      2.31
_cell_volume                     5134.4(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            62831
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.621
_diffrn_reflns_theta_min         1.542
_exptl_absorpt_coefficient_mu    3.676
_exptl_absorpt_correction_T_max  0.718
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.698
_refine_diff_density_min         -3.209
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         15733
_refine_ls_number_restraints     563
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+57.7758P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11661
_reflns_number_total             15733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00686_si_002.cif
_cod_data_source_block           dg261_6a
_cod_database_code               4347842
_shelxl_version_number           2012-9
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.646
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.021) H6(0.027) H8(0.027) H10A(0.05) H10B(0.05) H10C(0.05)
 H11A(0.055) H11B(0.055) H11C(0.055) H12A(0.037) H12B(0.037) H12C(0.037)
 H15(0.03) H17(0.028) H19A(0.036) H19B(0.036) H19C(0.036) H20A(0.058)
 H20B(0.058) H20C(0.058) H21A(0.033) H21B(0.033) H21C(0.033) H22A(0.038)
 H22B(0.038) H23A(0.035) H23B(0.035) H24A(0.048) H24B(0.048) H25A(0.051)
 H25B(0.051) H28(0.027) H30(0.03) H32A(0.04) H32B(0.04) H32C(0.04) H33A(0.055)
 H33B(0.055) H33C(0.055) H34A(0.034) H34B(0.034) H34C(0.034) H35(0.018)
 H37(0.03) H38(0.039) H39(0.04) H40(0.039) H41(0.03) H43(0.027) H44(0.031)
 H45(0.032) H46(0.03) H47(0.023) H48A(0.047) H48B(0.047) H49A(0.057)
 H49B(0.057) H22C(0.034) H22D(0.034) H23C(0.035) H23D(0.035) H24C(0.035)
 H24D(0.035) H25C(0.025) H25D(0.025)
 Fixed X: H2(0.333) H6(0.0163) H8(0.0642) H10A(0.1688) H10B(0.1216)
 H10C(0.0544) H11A(-0.0888) H11B(-0.0402) H11C(0.0095) H12A(0.1647)
 H12B(0.1396) H12C(0.2405) H15(0.2472) H17(0.254) H19A(0.264) H19B(0.2756)
 H19C(0.1699) H20A(0.1861) H20B(0.2594) H20C(0.3008) H21A(0.2365) H21B(0.2106)
 H21C(0.3216) H22A(-0.1632) H22B(-0.2302) H23A(-0.3424) H23B(-0.3067) H24A(-
 0.3002) H24B(-0.1986) H25A(-0.2489) H25B(-0.1552) H28(0.589) H30(0.523)
 H32A(0.5649) H32B(0.532) H32C(0.452) H33A(0.5741) H33B(0.6768) H33C(0.6371)
 H34A(0.3898) H34B(0.4015) H34C(0.4864) H35(0.5307) H37(0.6451) H38(0.8016)
 H39(0.8859) H40(0.8132) H41(0.659) H43(0.4728) H44(0.4434) H45(0.4509)
 H46(0.4888) H47(0.524) H48A(0.2556) H48B(0.3319) H49A(0.551) H49B(0.5505)
 H22C(-0.1585) H22D(-0.2509) H23C(-0.3141) H23D(-0.2113) H24C(-0.3012) H24D(-
 0.3325) H25C(-0.2093) H25D(-0.1458)
 Fixed Y: H2(0.2283) H6(0.2314) H8(0.0699) H10A(0.3353) H10B(0.327)
 H10C(0.3452) H11A(0.0919) H11B(0.1305) H11C(0.0656) H12A(0.1468) H12B(0.077)
 H12C(0.1116) H15(0.3575) H17(0.5105) H19A(0.2342) H19B(0.2468) H19C(0.2466)
 H20A(0.5085) H20B(0.4622) H20C(0.5192) H21A(0.4187) H21B(0.4887) H21C(0.4667)
 H22A(0.342) H22B(0.3943) H23A(0.3188) H23B(0.2883) H24A(0.2108) H24B(0.2178)
 H25A(0.279) H25B(0.2341) H28(0.5068) H30(0.4947) H32A(0.3672) H32B(0.4391)
 H32C(0.3855) H33A(0.6097) H33B(0.5767) H33C(0.5781) H34A(0.3516) H34B(0.4196)
 H34C(0.3664) H35(0.2816) H37(0.1759) H38(0.1894) H39(0.287) H40(0.369)
 H41(0.3536) H43(0.1535) H44(0.0459) H45(0.0131) H46(0.0897) H47(0.1974)
 H48A(0.046) H48B(0.0923) H49A(-0.0022) H49B(0.0734) H22C(0.4054) H22D(0.3738)
 H23C(0.3878) H23D(0.375) H24C(0.2798) H24D(0.278) H25C(0.2034) H25D(0.2459)
 Fixed Z: H2(0.8668) H6(0.9555) H8(0.8461) H10A(0.8893) H10B(0.9575)
 H10C(0.8718) H11A(0.9076) H11B(0.9869) H11C(0.9686) H12A(0.7184) H12B(0.7464)
 H12C(0.7911) H15(0.4767) H17(0.618) H19A(0.6175) H19B(0.5339) H19C(0.5441)
 H20A(0.4546) H20B(0.4291) H20C(0.4907) H21A(0.7786) H21B(0.7387) H21C(0.7746)
 H22A(0.7098) H22B(0.651) H23A(0.5911) H23B(0.677) H24A(0.5753) H24B(0.6439)
 H25A(0.4938) H25B(0.5326) H28(0.7354) H30(0.9333) H32A(0.6678) H32B(0.6365)
 H32C(0.6367) H33A(0.8416) H33B(0.8494) H33C(0.9223) H34A(0.8958) H34B(0.9409)
 H34C(0.9661) H35(0.9074) H37(0.8067) H38(0.7991) H39(0.8413) H40(0.8932)
 H41(0.9042) H43(0.7595) H44(0.7847) H45(0.9093) H46(1.0103) H47(0.9863)
 H48A(0.4836) H48B(0.5439) H49A(0.695) H49B(0.6737) H22C(0.576) H22D(0.5121)
 H23C(0.611) H23D(0.6765) H24C(0.6712) H24D(0.5783) H25C(0.6114) H25D(0.6844)
;
_shelx_res_checksum              81116
_shelx_hkl_checksum              26068
_olex2_submission_special_instructions 'No special instructions were received'