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_7049743
_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 Cu N2 O4 P4, C7 H8'
_chemical_formula_sum            'C75 H58 Cu N2 O4 P4'
_chemical_formula_weight         1238.65
_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             2017-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-06-07 deposited with the CCDC.    2019-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                84.797(4)
_cell_angle_beta                 79.338(4)
_cell_angle_gamma                84.311(4)
_cell_formula_units_Z            2
_cell_length_a                   11.2383(5)
_cell_length_b                   15.6851(7)
_cell_length_c                   17.5534(10)
_cell_measurement_reflns_used    19217
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.17
_cell_volume                     3017.5(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 0.996
_diffrn_measured_fraction_theta_max 0.980
_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  0.0432
_diffrn_reflns_av_unetI/netI     0.0701
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25887
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.840
_diffrn_reflns_theta_min         2.175
_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    0.523
_exptl_absorpt_correction_T_max  0.9979
_exptl_absorpt_correction_T_min  0.9510
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE Xred and LANA'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       plate
_exptl_crystal_F_000             1286
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         12702
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0796P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8370
_reflns_number_total             12702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05003a2.cif
_cod_data_source_block           wyx225_repeat
_cod_database_code               7049743
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.859
_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. Restrained distances
 C75B-C70B = C71B-C70B = C72B-C71B = C73B-C72B = C74B-C73B = C75B-C74B
 1.39 with sigma of 0.01
 C70A-C69A = C70B-C69B
 1.54 with sigma of 0.02
 C71A-C70A = C72A-C71A = C73A-C72A = C74A-C73A = C75A-C74A = C75A-C70A
 1.39 with sigma of 0.01
3. Others
 Fixed Sof: C69A(0.5) H69A(0.5) H69B(0.5) H69C(0.5) C70A(0.5) C71A(0.5)
 H71A(0.5) C72A(0.5) H72A(0.5) C73A(0.5) H73A(0.5) C74A(0.5) H74A(0.5)
 C75A(0.5) H75A(0.5) C69B(0.5) H69D(0.5) H69E(0.5) H69F(0.5) C70B(0.5)
 C71B(0.5) H71B(0.5) C72B(0.5) H72B(0.5) C73B(0.5) H73B(0.5) C74B(0.5)
 H74B(0.5) C75B(0.5) H75B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C2AA(H2AA), C2BA(H2BA), C3(H3), C3AA(H3AA), C4(H4), C5(H5),
 C5AA(H5AA), C6(H6), C7AA(H7AA), 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), 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), C71A(H71A), C72A(H72A),
 C73A(H73A), C74A(H74A), C75A(H75A), C71B(H71B), C72B(H72B), C73B(H73B),
 C74B(H74B), C75B(H75B)
4.b Idealised Me refined as rotating group:
 C69A(H69A,H69B,H69C), C69B(H69D,H69E,H69F)
;
_shelx_res_checksum              31620
_olex2_submission_special_instructions 'No special instructions were received'