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_7049754
_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
'C34 H25 Cl2 N O2 P2 Pd, 0.917(C6 H12), 0.25(C H2 Cl2)'
_chemical_formula_sum            'C39.75 H36.5 Cl2.5 N O2 P2 Pd'
_chemical_formula_weight         817.16
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-02
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   37.7119(13)
_cell_length_b                   37.7119(13)
_cell_length_c                   13.4414(4)
_cell_measurement_reflns_used    34159
_cell_measurement_temperature    133.15
_cell_measurement_theta_max      33.07
_cell_measurement_theta_min      1.87
_cell_volume                     16555.1(9)
_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      133.15
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.972
_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  0.0615
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21904
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.105
_diffrn_reflns_theta_min         1.871
_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    0.809
_exptl_absorpt_correction_T_max  0.6912
_exptl_absorpt_correction_T_min  0.2364
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE Xred and LANA'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       block
_exptl_crystal_F_000             7497
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.654
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     850
_refine_ls_number_reflns         13281
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0628
_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^)+(0.1128P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1584
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.972
_reflns_number_gt                11200
_reflns_number_total             13281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05003a2.cif
_cod_data_source_block           wyx032-1
_cod_original_cell_volume        16555.1(12)
_cod_original_formula_sum        'C39.75 H36.50 Cl2.50 N O2 P2 Pd'
_cod_database_code               7049754
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.55(4)
 0.45(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C70B-C71B = C71B-C72B = C72B-C73B = C73B-C74B = C69B-C74B = C69B-C70B
 1.54 with sigma of 0.02
 C74A-C69A = C74A-C73A = C73A-C72A = C72A-C71A = C71A-C70A = C70A-C69A
 1.54 with sigma of 0.02
 Cl5-C77 = Cl6-C77
 1.76 with sigma of 0.02
 C82-C81 = C80-C81 = C80-C79 = C79-C78 = C78-C83 = C83-C82
 1.54 with sigma of 0.02
 C83-C81
 2.51 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C74B \\sim C74B \\sim C74B \\sim C73B \\sim C73B \\sim C73B \\sim C72B \\sim
C72B \\sim C72B \\sim C71B \\sim C71B \\sim C71B \\sim C70B \\sim C70B \\sim
C70B \\sim C69B \\sim C69B \\sim C69B: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C78 \\sim C79 \\sim C83 \\sim C80 \\sim C82 \\sim C81 \\sim C79 \\sim C78 \\sim
C83 \\sim C78 \\sim C80 \\sim C79 \\sim C83 \\sim C82 \\sim C81 \\sim C80 \\sim
C82 \\sim C81: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
5. Others
 Fixed Sof: C69A(0.5) H69A(0.5) H69B(0.5) C70A(0.5) H70A(0.5) H70B(0.5)
 C71A(0.5) H71A(0.5) H71B(0.5) C72A(0.5) H72A(0.5) H72B(0.5) C73A(0.5)
 H73A(0.5) H73B(0.5) C74A(0.5) H74A(0.5) H74B(0.5) Cl6(0.5) C77(0.5) H77A(0.5)
 H77B(0.5) Cl5(0.5) C74B(0.5) H74C(0.5) H74D(0.5) C73B(0.5) H73C(0.5) H73D(0.5)
 C72B(0.5) H72C(0.5) H72D(0.5) C71B(0.5) H71C(0.5) H71D(0.5) C70B(0.5)
 H70C(0.5) H70D(0.5) C69B(0.5) H69C(0.5) H69D(0.5) C78(0.5) H78A(0.5) H78B(0.5)
 C79(0.5) H79A(0.5) H79B(0.5) C82(0.5) H82A(0.5) H82B(0.5) C83(0.5) H83A(0.5)
 H83B(0.5) C80(0.5) H80A(0.5) H80B(0.5) C81(0.5) H81A(0.5) H81B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C69A(H69A,H69B), C70A(H70A,H70B), C71A(H71A,H71B), C72A(H72A,H72B), C73A(H73A,
 H73B), C74A(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B),
 C74B(H74C,H74D), C73B(H73C,H73D), C72B(H72C,H72D), C71B(H71C,H71D), C70B(H70C,
 H70D), C69B(H69C,H69D), C78(H78A,H78B), C79(H79A,H79B), C82(H82A,H82B),
 C83(H83A,H83B), C80(H80A,H80B), C81(H81A,H81B)
6.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              50651
_olex2_submission_special_instructions 'No special instructions were received'