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_7049752
_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 Ag N2 O4 P4, C7 H8'
_chemical_formula_sum            'C75 H58 Ag N2 O4 P4'
_chemical_formula_weight         1282.98
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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     dual
_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                78.636(3)
_cell_angle_beta                 74.660(3)
_cell_angle_gamma                83.840(3)
_cell_formula_units_Z            3
_cell_length_a                   14.3361(5)
_cell_length_b                   15.8794(6)
_cell_length_c                   21.5123(7)
_cell_measurement_reflns_used    30520
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      1.78
_cell_volume                     4622.3(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    'ShelXD (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 0.991
_diffrn_measured_fraction_theta_max 0.984
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.0956
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37445
_diffrn_reflns_point_group_measured_fraction_full 0.780
_diffrn_reflns_point_group_measured_fraction_max 0.771
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.645
_diffrn_reflns_theta_min         1.862
_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    0.485
_exptl_absorpt_correction_T_max  0.9629
_exptl_absorpt_correction_T_min  0.8844
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRed and LANA'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       plate
_exptl_crystal_F_000             1983
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.011(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2228
_refine_ls_number_reflns         27013
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0332P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.568
_reflns_Friedel_fraction_full    0.568
_reflns_Friedel_fraction_max     0.559
_reflns_number_gt                19530
_reflns_number_total             27013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05003a2.cif
_cod_data_source_block           wyx038-red
_cod_database_code               7049752
_shelx_shelxl_version_number     2014/7
_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
 C221-C220 = C222-C221 = C223-C222 = C224-C223 = C225-C224 = C225-C220
 1.39 with sigma of 0.02
 C212-C213 = C219-C220 = C205-C206 = C19B-C20B
 1.54 with sigma of 0.01
3. Others
 Fixed Sof: C42A(0.6) H42A(0.6) C43A(0.6) H43A(0.6) C44A(0.6) H44A(0.6)
 C45A(0.6) H45A(0.6) C46A(0.6) H46A(0.6) C42B(0.4) H42B(0.4) C43B(0.4)
 H43B(0.4) C44B(0.4) H44B(0.4) C45B(0.4) H45B(0.4) C46B(0.4) H46B(0.4)
 C172(0.5) H172(0.5) C173(0.5) H173(0.5) C174(0.5) H174(0.5) C175(0.5)
 H175(0.5) C176(0.5) H176(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) C76B(0.5) H76B(0.5) C219(0.6)
 H21D(0.6) H21E(0.6) H21F(0.6) C220(0.6) C221(0.6) H221(0.6) C222(0.6)
 H222(0.6) C223(0.6) H223(0.6) C224(0.6) H224(0.6) C225(0.6) H225(0.6)
 C19B(0.4) H19A(0.4) H19B(0.4) H19C(0.4) C20B(0.4) C25B(0.4) H25B(0.4)
 C24B(0.4) H24B(0.4) C23B(0.4) H23B(0.4) C22B(0.4) H22B(0.4) C21B(0.4) H21G(0.4)
4.a 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), C42A(H42A),
 C43A(H43A), C44A(H44A), C45A(H45A), C46A(H46A), C42B(H42B), C43B(H43B),
 C44B(H44B), C45B(H45B), C46B(H46B), 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), C70(H70), C71(H71), C72(H72), C73(H73),
 C74(H74), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C86(H86), C87(H87),
  C88(H88), C89(H89), C90(H90), C92(H92), C93(H93), C94(H94), C95(H95),
 C96(H96), C98(H98), C99(H99), C100(H100), C101(H101), C102(H102), C104(H104),
 C105(H105), C106(H106), C107(H107), C108(H108), C110(H110), C111(H111),
 C112(H112), C113(H113), C114(H114), C120(H120), C121(H121), C122(H122),
 C123(H123), C124(H124), C126(H126), C127(H127), C128(H128), C129(H129),
 C130(H130), C132(H132), C133(H133), C134(H134), C135(H135), C136(H136),
 C138(H138), C139(H139), C140(H140), C141(H141), C142(H142), C144(H144),
 C145(H145), C146(H146), C147(H147), C148(H148), C154(H154), C155(H155),
 C156(H156), C157(H157), C158(H158), C160(H160), C161(H161), C162(H162),
 C163(H163), C164(H164), C166(H166), C167(H167), C168(H168), C169(H169),
 C170(H170), C172(H172), C173(H173), C174(H174), C175(H175), C176(H176),
 C72B(H72B), C73B(H73B), C74B(H74B), C75B(H75B), C76B(H76B), C178(H178),
 C179(H179), C180(H180), C181(H181), C182(H182), C188(H188), C189(H189),
 C190(H190), C191(H191), C192(H192), C194(H194), C195(H195), C196(H196),
 C197(H197), C198(H198), C200(H200), C201(H201), C202(H202), C203(H203),
 C204(H204), C207(H207), C208(H208), C209(H209), C210(H210), C211(H211),
 C214(H214), C215(H215), C216(H216), C217(H217), C218(H218), C221(H221),
 C222(H222), C223(H223), C224(H224), C225(H225), C25B(H25B), C24B(H24B),
 C23B(H23B), C22B(H22B), C21B(H21G)
4.b Fitted hexagon refined as free rotating group:
 C20B(C25B,C24B,C23B,C22B,C21B)
4.c Idealised Me refined as rotating group:
 C205(H20A,H20B,H20C), C212(H21A,H21B,H21C), C219(H21D,H21E,H21F), C19B(H19A,
 H19B,H19C)
;
_shelx_res_checksum              13410
_olex2_submission_special_instructions 'No special instructions were received'