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_7049759
_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, F6 P, 2.5(C H2 Cl2)'
_chemical_formula_sum            'C70.5 H55 Au Cl5 F6 N2 O4 P5'
_chemical_formula_weight         1637.23
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-06-07 deposited with the CCDC.    2019-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.168(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3809(3)
_cell_length_b                   28.6900(6)
_cell_length_c                   19.3683(5)
_cell_measurement_reflns_used    154068
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      2.14
_cell_volume                     7064.8(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 0.841
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.841
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            73930
_diffrn_reflns_point_group_measured_fraction_full 0.841
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.596
_diffrn_reflns_theta_min         2.140
_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_target            Mo
_diffrn_source_type              'sealed X-ray tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.450
_exptl_absorpt_correction_T_max  0.6766
_exptl_absorpt_correction_T_min  0.3855
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE LANA and Xred'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       needle
_exptl_crystal_F_000             3268
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.297
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.374
_refine_diff_density_min         -3.201
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         11170
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.290
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0932
_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          0.2659
_refine_ls_wR_factor_ref         0.2817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9721
_reflns_number_total             11170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05003a2.cif
_cod_data_source_block           wyx099-1
_cod_original_formula_sum        'C70.50 H55 Au Cl5 F6 N2 O4 P5'
_cod_database_code               7049759
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl3-C69A = Cl4A-C69A = Cl4B-C69B
 1.72 with sigma of 0.02
 Cl3-C69B
 1.72 with sigma of 0.02
3. Others
 Fixed Sof: Cl4A(0.7) C69A(0.7) H69A(0.7) H69B(0.7) Cl4B(0.3) C69B(0.3)
 H69C(0.3) H69D(0.3) Cl5(0.5) Cl6(0.5) C70(0.5) H70A(0.5) H70B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C68(H68A,H68B), C69A(H69A,H69B), C69B(H69C,H69D), C70(H70A,H70B)
4.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), C41(H41), C42(H42),
  C43(H43), C44(H44), C45(H45), C51(H51), C52(H52), C53(H53), C54(H54),
 C55(H55), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C63(H63), C64(H64),
  C65(H65), C66(H66), C67(H67)
;
_shelx_res_checksum              56233
_olex2_submission_special_instructions 'No special instructions were received'