Synthesis of New Chiral Bidentate Isonitrile‒Acyclic Diaminocarbene Palladium(II) Compounds and Their Catalytic Activity
Knorn, Matthias; Lutsker, Eugen; Reiser, Oliver; Organometallics 34 (2015) 4515–; doi:10.1021/acs.organomet.5b00516

data_4086256
_publ_section_title
;
 Synthesis of New Chiral Bidentate Isonitrile--Acyclic Diaminocarbene
 Palladium(II) Compounds and Their Catalytic Activity
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4515
_journal_paper_doi               10.1021/acs.organomet.5b00516
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H52 Cl2 N3 O3 P Pd'
_chemical_formula_sum            'C32 H52 Cl2 N3 O3 P Pd'
_chemical_formula_weight         735.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-04-21
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.6935(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.56244(16)
_cell_length_b                   17.2200(3)
_cell_length_c                   10.7458(2)
_cell_measurement_reflns_used    4057
_cell_measurement_temperature    122.98(17)
_cell_measurement_theta_max      70.2480
_cell_measurement_theta_min      4.1120
_cell_volume                     1760.73(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      122.98(17)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details
;
  1 omega -117.00  -17.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -37.0000   30.0000 200

  2 omega    2.00   98.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064 -125.0000    0.0000 192

  3 omega   33.00   76.00   0.5000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429  -45.0000   60.0000 86

  4 omega   34.00  121.00   0.5000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429 -125.0000  120.0000 174

  5 omega   46.00   77.00   0.5000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429  -45.0000   90.0000 62

  6 omega   74.00  144.00   0.5000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429   45.0000 -150.0000 140

  7 omega   28.00  158.00   0.5000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429    0.0000    0.0000 260

  8 omega -115.00  -12.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -57.0000  150.0000 206

  9 omega -120.00   -8.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -77.0000  -60.0000 224

 10 omega   23.00   48.00   0.5000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429  -30.0000 -180.0000 50
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1502767000
_diffrn_orient_matrix_UB_12      -0.0222067000
_diffrn_orient_matrix_UB_13      0.0266341000
_diffrn_orient_matrix_UB_21      0.0355713000
_diffrn_orient_matrix_UB_22      0.0212622000
_diffrn_orient_matrix_UB_23      0.1388687000
_diffrn_orient_matrix_UB_31      -0.0488905000
_diffrn_orient_matrix_UB_32      0.0839213000
_diffrn_orient_matrix_UB_33      -0.0279663000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_laue_measured_fraction_full 0.978
_diffrn_reflns_laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7961
_diffrn_reflns_point_group_measured_fraction_full 0.743
_diffrn_reflns_point_group_measured_fraction_max 0.718
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         70.857
_diffrn_reflns_theta_min         4.134
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.350
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.585
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       needle
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.1821
_exptl_crystal_size_mid          0.0199
_exptl_crystal_size_min          0.0104
_refine_diff_density_max         1.044
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 1330 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4862
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0554P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1008
_reflns_Friedel_coverage         0.450
_reflns_friedel_fraction_full    0.490
_reflns_friedel_fraction_max     0.461
_reflns_number_gt                4555
_reflns_number_total             4862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00516_si_003.cif
_cod_data_source_block           m065
_cod_database_code               4086256
_chemical_oxdiff_formula         'C32 H52 N3 O3 P1 Pd1 Cl2'
_reflns_odcompleteness_completeness 98.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C15(H15), C21(H21), C27(H27)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B),
 C25(H25A,H25B), C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
  C31(H31A,H31B), C32(H32A,H32B)
2.c Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
2.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), N2(H2A)
;
_shelx_res_checksum              79250
_shelx_hkl_checksum              78670
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'