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_4087940
_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         'C38 H30 N2 P2, 2(Cl)'
_chemical_formula_sum            'C38 H30 Cl2 N2 P2'
_chemical_formula_weight         647.48
_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             2015-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.922(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5972(3)
_cell_length_b                   14.7429(3)
_cell_length_c                   18.6732(4)
_cell_measurement_reflns_used    6367
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      72.0580
_cell_measurement_theta_min      4.3460
_cell_volume                     3844.57(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -61.00  -35.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  -60.0000 26

  2 omega   -4.00   42.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  150.0000 46

  3 omega  -21.00   23.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   30.0000    0.0000 44

  4 omega  -46.00   26.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   37.0000 -180.0000 72

  5 omega  -86.00   24.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   19.0000  120.0000 110

  6 omega   18.00  110.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -125.0000 -150.0000 92

  7 omega   39.00   64.00   1.0000   41.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -150.0000 25

  8 omega   40.00   89.00   1.0000   41.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -90.0000 49

  9 omega   43.00   70.00   1.0000   41.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  150.0000 27

 10 omega   93.00  174.00   1.0000   41.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   90.0000 81

 11 omega   39.00   90.00   1.0000   41.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -30.0000 51

 12 omega  135.00  168.00   1.0000   41.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000    0.0000 33

 13 omega  134.00  178.00   1.0000   41.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   30.0000 44

 14 omega   40.00   66.00   1.0000   41.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -60.0000 26

 15 omega   43.00   95.00   1.0000   41.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  120.0000 52

 16 omega   90.00  178.00   1.0000   41.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000 -180.0000 88

 17 omega  -30.00   70.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -150.0000 100

 18 omega   30.00   78.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   37.0000   60.0000 48
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0308907000
_diffrn_orient_matrix_UB_12      0.0508710000
_diffrn_orient_matrix_UB_13      -0.0612506000
_diffrn_orient_matrix_UB_21      0.0900786000
_diffrn_orient_matrix_UB_22      0.0347868000
_diffrn_orient_matrix_UB_23      0.0594350000
_diffrn_orient_matrix_UB_31      0.0555460000
_diffrn_orient_matrix_UB_32      -0.0844778000
_diffrn_orient_matrix_UB_33      -0.0124085000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14192
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.065
_diffrn_reflns_theta_max         67.065
_diffrn_reflns_theta_min         3.165
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.499
_exptl_absorpt_correction_type   none
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         2.833
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.117
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6861
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0836
_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^)+(0.1865P)^2^+1.5223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2442
_refine_ls_wR_factor_ref         0.2617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5418
_reflns_number_total             6861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00746_si_006.cif
_cod_data_source_block           201506156
_cod_database_code               4087940
_chemical_oxdiff_formula         C20H20N4O4P2Cl1
_shelx_estimated_absorpt_t_max   0.788
_shelx_estimated_absorpt_t_min   0.662
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N2-H2A
 0.95 with sigma of 0.02
 N1-H1
 0.95 with sigma of 0.02
3.a 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), C23(H23), C24(H24), C25(H25),
  C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34),
 C35(H35), C36(H36), C37(H37), C38(H38)
;
_shelx_res_checksum              7258
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'