Making the Unconventional μ2-P Bridging Binding Mode More Conventional in Phosphinine Complexes
Gruetzmacher, Hansjoerg; Hou, Yuanfeng; Li, Zhongshu; Li, Yaqi; Su, Cheng-Yong; Puschmann, Florian; Liu, Peng; Chemical Science  (2019) –; doi:10.1039/C8SC05281F

data_1550497
_publ_section_title
;
 Making the Unconventional \m2-P Bridging Binding Mode More Conventional
 in Phosphinine Complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC05281F
_journal_year                    2019
_chemical_formula_moiety         'C87 H66 Au6 Cl O5 P5 S, 2(C H2 Cl2), C3 H7'
_chemical_formula_sum            'C92 H77 Au6 Cl5 O5 P5 S'
_chemical_formula_weight         2808.49
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-10-09 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.0770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.31190(10)
_cell_length_b                   21.8107(2)
_cell_length_c                   28.8693(2)
_cell_measurement_reflns_used    108189
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.8940
_cell_measurement_theta_min      3.5660
_cell_volume                     9520.55(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -89.00  17.00   0.50    2.00    --    0.00 -38.00   0.00  212
  2  \w    -17.00  89.00   0.50    2.00    --    0.00  38.00 -30.00  212
  3  \w    -89.00  17.00   0.50    2.00    --    0.00 -38.00-180.00  212
  4  \w    -89.00  17.00   0.50    2.00    --    0.00 -38.00  90.00  212
  5  \w    -17.00  89.00   0.50    2.00    --    0.00  38.00-180.00  212
  6  \w    -29.00  89.00   0.50    2.00    --    0.00  77.00  60.00  236
  7  \w    -17.00  89.00   0.50    2.00    --    0.00  38.00-120.00  212
  8  \w     71.00 185.00   0.50   10.00    --   95.20  65.00-150.21  228
  9  \w      6.00 119.00   0.50   10.00    --   95.20 -15.00 -90.00  226
 10  \w      6.00 119.00   0.50   10.00    --   95.20 -61.00  60.00  226
 11  \w      6.00 127.00   0.50   10.00    --   95.20 -82.00 -90.00  242
 12  \w      6.00 127.00   0.50   10.00    --   95.20 -82.00  60.00  242
 13  \w      6.00 127.00   0.50   10.00    --   95.20 -82.00 120.00  242
 14  \w     79.00 185.00   0.50   10.00    --   95.20  30.00 -90.00  212
 15  \w      6.00 127.00   0.50   10.00    --   95.20 -82.00   0.00  242
 16  \w      6.00 119.00   0.50   10.00    --   95.20 -61.00-180.00  226
 17  \w     79.00 185.00   0.50   10.00    --   95.20  30.00 -60.00  212
 18  \w      6.00 115.00   0.50   10.00    --   95.20 -45.00 120.00  218
 19  \w      6.00 127.00   0.50   10.00    --   95.20 -82.00-150.00  242
 20  \w      6.00 127.00   0.50   10.00    --   95.20 -82.00-180.00  242
 21  \w      6.00 119.00   0.50   10.00    --   95.20 -61.00 -60.00  226
 22  \w      6.00 112.00   0.50   10.00    --   95.20 -30.00 -90.00  212
 23  \w    -31.00  89.00   0.50    2.00    --    0.00  82.00  90.00  240
 24  \w    -31.00  48.00   0.50    2.00    --    0.00  82.00 150.00  158
 25  \w    -89.00  22.00   0.50    2.00    --    0.00 -57.00-120.00  222
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0729985000
_diffrn_orient_matrix_UB_12      0.0350615000
_diffrn_orient_matrix_UB_13      0.0322736000
_diffrn_orient_matrix_UB_21      0.0660152000
_diffrn_orient_matrix_UB_22      -0.0519120000
_diffrn_orient_matrix_UB_23      -0.0053579000
_diffrn_orient_matrix_UB_31      0.0263437000
_diffrn_orient_matrix_UB_32      0.0327194000
_diffrn_orient_matrix_UB_33      -0.0429783000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            170600
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.451
_diffrn_reflns_theta_min         2.551
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.613
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_description       block
_exptl_crystal_F_000             5276
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         3.334
_refine_diff_density_min         -1.701
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1000
_refine_ls_number_reflns         19015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0666
_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^)+(0.0564P)^2^+341.5175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1710
_refine_ls_wR_factor_ref         0.1722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17794
_reflns_number_total             19015
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05281f2.cif
_cod_data_source_block           exp_97
_cod_database_code               1550497
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.145
_shelx_estimated_absorpt_t_min   0.111
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C34) = Uanis(C33) = Uanis(C32) = Uanis(C31) = Uanis(C30) = Uanis(C29)
3.a Secondary CH2 refined with riding coordinates:
 C7BA(H7BA,H7BB), C3AA(H3AA,H3AB), C7AA(H7AA,H7AB), C1BA(H1BA,H1BB)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C11(H11), C75(H75), C2(H2), C72(H72), C17(H17), C7(H7), C51(H51),
 C9(H9), C42(H42), C16(H16), C70(H70), C50(H50), C82(H82), C19(H19), C83(H83),
 C53(H53), C79(H79), C78(H78), C47(H47), C55(H55), C81(H81), C8(H8), C48(H48),
 C10(H10), C13(H13), C49(H49), C64(H64), C85(H85), C84(H84), C67(H67), C21(H21),
  C76(H76), C28(H28), C27(H27), C43(H43), C77(H77), C15(H15), C66(H66),
 C57(H57), C68(H68), C24(H24), C58(H58), C25(H25), C26(H26), C45(H45), C61(H61),
  C14(H14), C33(H33), C44(H44), C65(H65), C59(H59), C34(H34), C30(H30),
 C32(H32), C38(H38), C41(H41), C36(H36), C60(H60), C31(H31)
3.c Idealised Me refined as rotating group:
 C8AA(H8AA,H8AB,H8AC), C0AA(H0AA,H0AB,H0AC), C6AA(H6AA,H6AB,H6AC)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.734
_oxdiff_exptl_absorpt_empirical_full_min 0.638