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_7049755
_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, 2.5(C H2 Cl2), F6 P'
_chemical_formula_sum            'C70.5 H55 Au Cl5 F6 N2 O4 P5'
_chemical_formula_weight         1637.23
_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             2017-10-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-06-07 deposited with the CCDC.    2019-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                95.619(3)
_cell_angle_beta                 108.526(3)
_cell_angle_gamma                97.034(3)
_cell_formula_units_Z            2
_cell_length_a                   13.3647(4)
_cell_length_b                   14.5914(7)
_cell_length_c                   19.3008(8)
_cell_measurement_reflns_used    45782
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      26.07
_cell_measurement_theta_min      1.98
_cell_volume                     3504.3(3)
_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                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.882
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_Laue_measured_fraction_full 0.882
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25374
_diffrn_reflns_point_group_measured_fraction_full 0.882
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.746
_diffrn_reflns_theta_min         2.237
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.469
_exptl_absorpt_correction_T_max  0.7769
_exptl_absorpt_correction_T_min  0.4707
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE Xred and LANA'
_exptl_crystal_colour            'bluish violet'
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       plate
_exptl_crystal_F_000             1634
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.070
_refine_diff_density_min         -2.908
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         11692
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0909
_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^)+(0.1952P)^2^+0.9972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2343
_refine_ls_wR_factor_ref         0.2672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8350
_reflns_number_total             11692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05003a2.cif
_cod_data_source_block           wyx080-1
_cod_original_formula_sum        'C70.50 H55 Au Cl5 F6 N2 O4 P5'
_cod_database_code               7049755
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl6-Cl5
 2.9 with sigma of 0.02
 Cl6-C71 = Cl5-C71
 1.76 with sigma of 0.02
 Cl4-C70B = Cl3B-C70B = Cl4-C70A = C70A-Cl3A
 1.76 with sigma of 0.02
 Cl4-Cl3B = Cl4-Cl3A
 2.9 with sigma of 0.02
 C62-C57
 1.39 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N15 \\sim C47 \\sim C50 \\sim C51: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uiso(Cl3A) = Uiso(C70A)
4. Others
 Fixed Sof: Cl5(0.5) Cl6(0.5) C71(0.5) H71A(0.5) H71B(0.5) Cl3A(0.2) C70A(0.2)
 H70A(0.2) H70B(0.2) C70B(0.8) H70C(0.8) H70D(0.8) Cl3B(0.8)
5.a Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C69(H69A,H69B), C70A(H70A,H70B), C70B(H70C,H70D)
5.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), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43),
  C44(H44), C45(H45), C46(H46), C52(H52), C53(H53), C54(H54), C55(H55),
 C56(H56), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C64(H64), C65(H65),
  C66(H66), C67(H67), C68(H68)
;
_shelx_res_checksum              85746
_olex2_submission_special_instructions 'No special instructions were received'