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_7049762
_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         'C34 H25 Cl2 N O2 P2 Pd, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C34.5 H26 Cl3 N O2 P2 Pd'
_chemical_formula_weight         761.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-09-21
_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                90
_cell_angle_beta                 111.516(4)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   27.3505(14)
_cell_length_b                   17.7863(13)
_cell_length_c                   27.8832(14)
_cell_measurement_reflns_used    145443
_cell_measurement_temperature    133.15
_cell_measurement_theta_max      33.58
_cell_measurement_theta_min      1.48
_cell_volume                     12619.0(13)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0263
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            88531
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.451
_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    0.978
_exptl_absorpt_correction_T_max  0.9311
_exptl_absorpt_correction_T_min  0.5807
_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    1.603
_exptl_crystal_description       needle
_exptl_crystal_F_000             6128
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1567
_refine_ls_number_reflns         24787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+5.8677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19811
_reflns_number_total             24787
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05003a2.cif
_cod_data_source_block           wyx032-1a
_cod_original_formula_sum        'C34.50 H26 Cl3 N O2 P2 Pd'
_cod_database_code               7049762
_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.a Secondary CH2 refined with riding coordinates:
 C138(H13A,H13B), C137(H13C,H13D)
2.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C42(H42), C18(H18), C25(H25), C80(H80), C96(H96), C70(H70),
 C114(H114), C108(H108), C136(H136), C12(H12), C135(H135), C126(H126), C11(H11),
  C113(H113), C76(H76), C132(H132), C105(H105), C134(H134), C104(H104),
 C77(H77), C79(H79), C73(H73), C74(H74), C133(H133), C110(H110), C71(H71),
 C62(H62), C28(H28), C88(H88), C89(H89), C94(H94), C8(H8), C68(H68), C93(H93),
 C87(H87), C90(H90), C86(H86), C65(H65), C58(H58), C95(H95), C112(H112),
 C92(H92), C111(H111), C106(H106), C59(H59), C78(H78), C10(H10), C64(H64),
 C9(H9), C60(H60), C26(H26), C52(H52), C34(H34), C6(H6), C54(H54), C53(H53),
 C45(H45), C46(H46), C33(H33), C55(H55), C40(H40), C30(H30), C56(H56), C66(H66),
  C37(H37), C44(H44), C5(H5), C39(H39), C38(H38), C36(H36), C27(H27), C2(H2),
 C67(H67), C21(H21), C20(H20), C120(H120), C127(H127), C124(H124), C22(H22),
 C32(H32), C19(H19), C31(H31), C129(H129), C4(H4), C61(H61), C3(H3), C128(H128),
  C130(H130), C102(H102), C98(H98), C122(H122), C123(H123), C121(H121),
 C43(H43), C107(H107), C101(H101), C99(H99), C100(H100), C72(H72)
;
_shelx_res_checksum              41823
_olex2_submission_special_instructions 'No special instructions were received'