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_4087942
_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         'C37 H30 Cl N2 P2 Pd, C H Cl3, Cl'
_chemical_formula_sum            'C38 H31 Cl5 N2 P2 Pd'
_chemical_formula_weight         861.24
_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   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2015-05-06
_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
_cell_angle_beta                 103.1612(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7584(2)
_cell_length_b                   16.6336(3)
_cell_length_c                   21.6767(3)
_cell_measurement_reflns_used    4614
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      68.9560
_cell_measurement_theta_min      3.3520
_cell_volume                     3777.18(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)
;
_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)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega   -3.00   30.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.5984   57.0000  -30.0000 33

  2 omega  -98.00  -61.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.5984 -153.0000  117.0000 37

  3 omega  -57.00  -32.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.5984  178.0000  -60.0000 25

  4 omega -106.00   -7.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.5984  -77.0000  -60.0000 99

  5 omega  -49.00   17.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.5984   37.0000  120.0000 66

  6 omega -113.00  -77.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.5984  178.0000  -60.0000 36

  7 omega   19.00   68.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5984  -99.0000  -90.0000 49

  8 omega   33.00   90.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5695  -30.0000   60.0000 57

  9 omega   35.00  103.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5695  -94.0000  -90.0000 68

 10 omega   33.00   96.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5695 -111.0000   90.0000 63

 11 omega   52.00   86.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5695  -30.0000  -60.0000 34

 12 omega  130.00  164.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5695  111.0000    0.0000 34

 13 omega   35.00   94.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5695  -45.0000 -120.0000 59

 14 omega   58.00   85.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5695  -30.0000   90.0000 27

 15 omega   80.00  108.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5695  -94.0000  -60.0000 28

 16 omega   89.00  168.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5695   61.0000 -150.0000 79

 17 omega   76.00  175.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5695   77.0000  -30.0000 99
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0473159000
_diffrn_orient_matrix_UB_12      -0.0679888000
_diffrn_orient_matrix_UB_13      0.0478336000
_diffrn_orient_matrix_UB_21      0.0721881000
_diffrn_orient_matrix_UB_22      0.0619153000
_diffrn_orient_matrix_UB_23      0.0477967000
_diffrn_orient_matrix_UB_31      -0.1192101000
_diffrn_orient_matrix_UB_32      0.0106050000
_diffrn_orient_matrix_UB_33      0.0274064000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14061
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.086
_diffrn_reflns_theta_max         67.086
_diffrn_reflns_theta_min         3.383
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.254
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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
;
;
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.405
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         6719
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0472
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5335
_reflns_number_total             6719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00746_si_005.cif
_cod_data_source_block           20150598
_cod_original_cell_volume        3777.18(12)
_cod_database_code               4087942
_chemical_oxdiff_formula         C20H20N4O4Cl1Pd1P1
_shelx_estimated_absorpt_t_max   0.492
_shelx_estimated_absorpt_t_min   0.334
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N2-H2A
 0.82 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C38(H38)
3.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), C21(H21), C22(H22), C23(H23),
  C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33),
 C34(H34), C35(H35), C36(H36), C37(H37)
;
_shelx_res_checksum              67755
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'