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_7049741
_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_absolute_configuration ad
_chemical_formula_moiety         'C76 H62 Cu4 N2 O12 P4, 2(C H2 Cl2)'
_chemical_formula_sum            'C78 H66 Cl4 Cu4 N2 O12 P4'
_chemical_formula_weight         1743.16
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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     direct
_audit_creation_date             2019-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-14 deposited with the CCDC.    2019-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                97.427(2)
_cell_angle_beta                 91.569(2)
_cell_angle_gamma                103.892(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6227(3)
_cell_length_b                   12.3603(3)
_cell_length_c                   27.4728(7)
_cell_measurement_reflns_used    163915
_cell_measurement_temperature    193.15
_cell_measurement_theta_max      30.47
_cell_measurement_theta_min      1.71
_cell_volume                     3792.16(17)
_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      193.15
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '4-circle goniometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            67389
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.772
_diffrn_source                   'Mo GeniX 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_target            Mo
_diffrn_source_type              'microfocus sealed X-ray tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.394
_exptl_absorpt_correction_T_max  0.8513
_exptl_absorpt_correction_T_min  0.7269
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Stoe Xred and LANA'
_exptl_crystal_colour            'brownish violet'
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.130(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1882
_refine_ls_number_reflns         31716
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0623
_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^)+(0.1317P)^2^+0.2068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1691
_refine_ls_wR_factor_ref         0.1759
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_full    0.936
_reflns_Friedel_fraction_max     0.918
_reflns_number_gt                28263
_reflns_number_total             31716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05003a2.cif
_cod_data_source_block           wxyo12-2a
_cod_database_code               7049741
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.870(11)
 0.130(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C155(H15A,H15B), C154(H15C,H15D), C153(H15E,H15F), C156(H15G,H15H)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
  C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C60(H60), C61(H61),
 C62(H62), C63(H63), C64(H64), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70),
  C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C86(H86), C87(H87),
 C88(H88), C89(H89), C90(H90), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96),
  C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C108(H108),
 C109(H109), C110(H110), C111(H111), C112(H112), C114(H114), C115(H115),
 C116(H116), C117(H117), C118(H118), C120(H120), C121(H121), C122(H122),
 C123(H123), C124(H124), C126(H126), C127(H127), C128(H128), C129(H129),
 C130(H130), C136(H136), C137(H137), C138(H138), C139(H139), C140(H140),
 C142(H142), C143(H143), C144(H144), C145(H145), C146(H146), C148(H148),
 C149(H149), C150(H150), C151(H151), C152(H152)
3.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C78(H78A,
 H78B,H78C), C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C84(H84A,H84B,H84C)
;
_shelx_res_checksum              19741
_olex2_submission_special_instructions 'No special instructions were received'