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_7049761
_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, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C35.5 H28 Cl5 N O2 P2 Pd'
_chemical_formula_weight         846.18
_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             2017-06-01
_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                77.447(7)
_cell_angle_beta                 76.796(6)
_cell_angle_gamma                71.073(7)
_cell_formula_units_Z            4
_cell_length_a                   11.3516(8)
_cell_length_b                   15.8507(15)
_cell_length_c                   21.6322(19)
_cell_measurement_reflns_used    8221
_cell_measurement_temperature    133.15
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      1.56
_cell_volume                     3540.9(5)
_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 0.879
_diffrn_measured_fraction_theta_max 0.874
_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  0.0938
_diffrn_reflns_av_unetI/netI     0.1672
_diffrn_reflns_Laue_measured_fraction_full 0.879
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17569
_diffrn_reflns_point_group_measured_fraction_full 0.879
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.375
_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    1.026
_exptl_absorpt_correction_T_max  0.8549
_exptl_absorpt_correction_T_min  0.6199
_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    1.587
_exptl_crystal_description       needle
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.291
_refine_diff_density_min         -1.474
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         12139
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.1428
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0875P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1617
_refine_ls_wR_factor_ref         0.1834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6584
_reflns_number_total             12139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05003a2.cif
_cod_data_source_block           wyx032-1b
_cod_original_cell_volume        3540.9(6)
_cod_original_formula_sum        'C35.50 H28 Cl5 N O2 P2 Pd'
_cod_database_code               7049761
_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. Uiso/Uaniso restraints and constraints
Uanis(C20) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.09
Uanis(Cl9) = Uanis(C71) = Uanis(Cl10)
3.a Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B)
3.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              38342
_olex2_submission_special_instructions 'No special instructions were received'