The coordination behavior of 2,3-bis(diphenylphosphino)maleic-N-phenylimide towards copper, silver, gold and palladium
Wang, Yingxia; Eichhoefer, Andreas; Weigend, Florian; Fenske, Dieter; Fuhr, Olaf; Dalton Transactions  (2019) –; doi:10.1039/C8DT05003A

data_7049748
_publ_section_title
;
 The coordination behavior of
 2,3-bis(diphenylphosphino)maleic-N-phenylimide towards copper, silver,
 gold and palladium
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT05003A
_journal_year                    2019
_chemical_formula_moiety         'C68 H50 Au N2 O4 P4, 2(C7 H8), Cl'
_chemical_formula_sum            'C82 H66 Au Cl N2 O4 P4'
_chemical_formula_weight         1499.66
_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     heavy
_audit_creation_date             2017-05-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-06-07 deposited with the CCDC.    2019-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                75.302(3)
_cell_angle_beta                 74.805(3)
_cell_angle_gamma                89.165(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6909(4)
_cell_length_b                   15.5366(5)
_cell_length_c                   20.1956(7)
_cell_measurement_reflns_used    23934
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      70.87
_cell_measurement_theta_min      5.20
_cell_volume                     3418.9(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.15
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device       '4-circle goniometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '2.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.912
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20533
_diffrn_reflns_point_group_measured_fraction_full 0.912
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         65.994
_diffrn_reflns_theta_min         5.196
_diffrn_source                   'Cu Genix 3D'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_target            Cu
_diffrn_source_type              'microfocus sealed X-ray tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.712
_exptl_absorpt_correction_T_max  0.7950
_exptl_absorpt_correction_T_min  0.3786
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE Xred and LANA'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       plate
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         5.623
_refine_diff_density_min         -2.273
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     852
_refine_ls_number_reflns         11271
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0905
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2356
_refine_ls_wR_factor_ref         0.2469
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9333
_reflns_number_total             11271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05003a2.cif
_cod_data_source_block           wyx110-1_dcm_tol
_cod_database_code               7049748
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C64(H64), C36(H36), C8(H8), C30(H30), C12(H12), C9(H9), C18(H18), C19(H19),
 C65(H65), C34(H34), C40(H40), C52(H52), C58(H58), C20(H20), C33(H33), C6(H6),
 C62(H62), C68(H68), C37(H37), C38(H38), C2(H2), C10(H10), C42(H42), C46(H46),
 C24(H24), C5(H5), C53(H53), C4(H4), C54(H54), C67(H67), C59(H59), C28(H28),
 C3(H3), C21(H21), C22(H22), C60(H60), C66(H66), C11(H11), C55(H55), C56(H56),
 C61(H61), C32(H32), C31(H31), C43(H43), C45(H45), C44(H44), C25(H25), C27(H27),
  C26(H26), C79(H79), C82(H82), C39(H39), C80(H80), C78(H78), C72(H72),
 C71(H71), C74(H74), C75(H75), C73(H73), C81(H81)
2.b Idealised Me refined as rotating group:
 C76(H76A,H76B,H76C), C69(H69A,H69B,H69C)
;
_shelx_res_checksum              61564
_olex2_submission_special_instructions 'No special instructions were received'