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_7049756
_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         'C68 H50 N2 O4 P4 Pd, C H2 Cl2'
_chemical_formula_sum            'C69 H52 Cl2 N2 O4 P4 Pd'
_chemical_formula_weight         1274.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2017-03-23
_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                 97.454(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.3882(11)
_cell_length_b                   11.1956(3)
_cell_length_c                   21.9982(9)
_cell_measurement_reflns_used    30528
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      2.18
_cell_volume                     5711.4(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0582
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25025
_diffrn_reflns_point_group_measured_fraction_full 0.919
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.177
_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    0.585
_exptl_absorpt_correction_T_max  0.9314
_exptl_absorpt_correction_T_min  0.8618
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Stoe XRed'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.276
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 3180 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_coef       0.00143(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         10274
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0729P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1211
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.839
_reflns_Friedel_fraction_max     0.833
_reflns_number_gt                8476
_reflns_number_total             10274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05003a2.cif
_cod_data_source_block           wyx-10_cyhex
_cod_database_code               7049756
_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
 Cl2B-C69B = Cl1B-C69B
 1.76 with sigma of 0.02
 H69A-H43_$1
 2.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(Cl1B) = Uiso(Cl2B) = Uiso(C69B)
4. Others
 Fixed Sof: C23A(0.5) C24A(0.5) H24A(0.5) C25A(0.5) H25A(0.5) C26A(0.5)
 H26A(0.5) C27A(0.5) H27A(0.5) C28A(0.5) H28A(0.5) Cl1B(0.25) Cl1A(0.75)
 Cl2A(0.75) C26B(0.5) H26B(0.5) C24B(0.5) H24B(0.5) C25B(0.5) H25B(0.5)
 C69A(0.75) H69C(0.75) H69D(0.75) C27B(0.5) H27B(0.5) C28B(0.5) H28B(0.5)
 Cl2B(0.25) C69B(0.25) H69A(0.25) H69B(0.25) C23B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C69A(H69C,H69D), C69B(H69A,H69B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
 C24A(H24A), C25A(H25A), C26A(H26A), C27A(H27A), C28A(H28A), C30(H30), C31(H31),
  C32(H32), C33(H33), C34(H34), C40(H40), C41(H41), C42(H42), C43(H43),
 C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), 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), C26B(H26B),
 C24B(H24B), C25B(H25B), C27B(H27B), C28B(H28B)
;
_shelx_res_checksum              93546
_olex2_submission_special_instructions 'No special instructions were received'