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_1550504
_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         'C35 H27 Au O P2'
_chemical_formula_sum            'C35 H27 Au O P2'
_chemical_formula_weight         722.47
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-10-09 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                87.576(4)
_cell_angle_beta                 84.280(4)
_cell_angle_gamma                71.512(4)
_cell_formula_units_Z            2
_cell_length_a                   10.7949(4)
_cell_length_b                   11.5285(6)
_cell_length_c                   11.9802(5)
_cell_measurement_reflns_used    4096
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      73.2400
_cell_measurement_theta_min      4.0270
_cell_volume                     1406.85(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.953
_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   -113.00 -17.00   1.00    2.00    --  -41.14 -38.00 -60.00   96
  2  \w    -74.00  25.00   1.00    1.00    --  -41.14  77.00-150.00   99
  3  \w    -65.00  27.00   1.00    1.00    --  -41.14  38.00 120.00   92
  4  \w     31.00 133.00   1.00    1.87    --  106.40 -30.00  60.00  102
  5  \w     84.00 110.00   1.00    1.87    --  106.40  30.00-120.00   26
  6  \w    128.00 178.00   1.00    1.87    --  106.40  30.00-120.00   50
  7  \w     43.00 135.00   1.00    1.87    --  106.40 -30.00 -90.00   92
  8  \w     47.00 109.00   1.00    1.87    --  106.40 -95.00-180.00   62
  9  \w     34.00 118.00   1.00    1.87    --  106.40 -77.00-120.00   84
 10  \w     67.00 134.00   1.00    1.87    --  106.40 -30.00-180.00   67
 11  \w     25.00 105.00   1.00    1.87    --  106.40 -95.00  90.00   80
 12  \w     60.00 118.00   1.00    1.87    --  106.40-119.00  41.00   58
 13  \w     30.00  62.00   1.00    1.87    --  106.40 -30.00-180.00   32
 14  \w    106.00 131.00   1.00    1.00    --   42.53 178.00-150.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0255649000
_diffrn_orient_matrix_UB_12      0.1382563000
_diffrn_orient_matrix_UB_13      0.0127829000
_diffrn_orient_matrix_UB_21      0.0079466000
_diffrn_orient_matrix_UB_22      -0.0181145000
_diffrn_orient_matrix_UB_23      0.1275381000
_diffrn_orient_matrix_UB_31      0.1487153000
_diffrn_orient_matrix_UB_32      -0.0203293000
_diffrn_orient_matrix_UB_33      -0.0165735000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0773
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8375
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.433
_diffrn_reflns_theta_min         3.708
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.107
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.309
_refine_diff_density_min         -1.533
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0680P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1281
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4812
_reflns_number_total             5385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05281f2.cif
_cod_data_source_block           exp_2681
_cod_database_code               1550504
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.435
_shelx_estimated_absorpt_t_min   0.326
_reflns_odcompleteness_completeness 99.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C19(H19), C29(H29), C4(H4), C20(H20), C25(H25), C10(H10), C22(H22),
 C23(H23), C12(H12), C2(H2), C31(H31), C35(H35), C16(H16), C6(H6), C28(H28),
 C26(H26), C32(H32), C13(H13), C15(H15), C14(H14), C7(H7), C9(H9), C27(H27),
 C8(H8), C33(H33), C34(H34)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.212
_oxdiff_exptl_absorpt_empirical_full_min 0.638