The Chemistry of ortho-(Diarylphosphino)aryl Isocyanides
Zhang, Lujun; Yu, Wenfei; Liu, Changchun; Xu, Youzhi; Duan, Zheng; Mathey, Francois; Organometallics 34 (2015) 5697–; doi:10.1021/acs.organomet.5b00746

data_4087941
_publ_section_title
;
 The Chemistry of ortho-(Diarylphosphino)aryl Isocyanides
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5697
_journal_paper_doi               10.1021/acs.organomet.5b00746
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C36 H32 Au2 N2 P2, 2(C F3 O3 S), 2(C H Cl3)'
_chemical_formula_sum            'C40 H34 Au2 Cl6 F6 N2 O6 P2 S2'
_chemical_formula_weight         1485.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-14
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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_cell_angle_alpha                90
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_cell_length_a                   9.9220(3)
_cell_length_b                   13.4139(3)
_cell_length_c                   18.8864(4)
_cell_measurement_reflns_used    3967
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      72.4760
_cell_measurement_theta_min      4.4610
_cell_volume                     2506.38(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
  1 omega   41.00   68.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 27

  2 omega  -11.00   16.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 27

  3 omega   16.00   42.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   30.0000 26

  4 omega   42.00   81.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -37.0000   90.0000 39

  5 omega  -16.00   12.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -37.0000   90.0000 28

  6 omega    2.00   67.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000 -150.0000 65

  7 omega   43.00  112.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000  -30.0000 69

  8 omega   73.00   99.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   37.0000  -60.0000 26

  9 omega   51.00  123.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000   60.0000 72

 10 omega   42.00   68.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -120.0000 26

 11 omega   50.00   84.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -90.0000 34

 12 omega   39.00   87.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   30.0000 48

 13 omega  116.00  175.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000   30.0000 59

 14 omega  120.00  170.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000 -180.0000 50

 15 omega  116.00  177.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  -30.0000 61

 16 omega  101.00  175.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000   60.0000 74

 17 omega   71.00   98.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  150.0000 27

 18 omega   39.00  176.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000    0.0000 -120.0000 137
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1552444000
_diffrn_orient_matrix_UB_12      0.0007576000
_diffrn_orient_matrix_UB_13      0.0128064000
_diffrn_orient_matrix_UB_21      -0.0054140000
_diffrn_orient_matrix_UB_22      -0.0993909000
_diffrn_orient_matrix_UB_23      0.0405980000
_diffrn_orient_matrix_UB_31      0.0112688000
_diffrn_orient_matrix_UB_32      -0.0575691000
_diffrn_orient_matrix_UB_33      -0.0698354000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9626
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.398
_diffrn_reflns_theta_min         4.046
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.777
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour
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_exptl_crystal_density_diffrn    1.968
_exptl_crystal_description
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_exptl_crystal_F_000             1424
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_exptl_crystal_size_mid          0.1
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_refine_diff_density_max         2.046
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0723P)^2^+0.6200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4066
_reflns_number_total             4848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00746_si_004.cif
_cod_data_source_block           201505106
_cod_original_cell_volume        2506.38(10)
_cod_database_code               4087941
_chemical_oxdiff_formula         C20H20N4O4P1S1F3Au1
_shelx_estimated_absorpt_t_max   0.506
_shelx_estimated_absorpt_t_min   0.216
_reflns_odcompleteness_completeness 99.94
_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 N(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17)
;
_shelx_res_checksum              75121
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'