Platinum(II) as an assembly point for carbide and nitride ligands
Reinholdt, Anders; Bendix, Jesper; Chemical Communications  (2019) –; doi:10.1039/C9CC03411K

data_7123716
_publ_section_title
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 Platinum(II) as an assembly point for carbide and nitride ligands
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03411K
_journal_year                    2019
_chemical_formula_moiety         'C67 H88 Cl4 Cr N O4 P2 Pt Ru'
_chemical_formula_sum            'C67 H88 Cl4 Cr N O4 P2 Pt Ru'
_chemical_formula_weight         1523.28
_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
_audit_creation_date             2018-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2019-05-01 deposited with the CCDC.    2019-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                88.0019(15)
_cell_angle_beta                 78.0480(14)
_cell_angle_gamma                82.9501(14)
_cell_formula_units_Z            6
_cell_length_a                   13.9110(6)
_cell_length_b                   23.2724(10)
_cell_length_c                   32.5218(13)
_cell_measurement_reflns_used    9482
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.062
_cell_measurement_theta_min      2.362
_cell_volume                     10222.1(7)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.899
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            325959
_diffrn_reflns_point_group_measured_fraction_full 0.899
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.168
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.672
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1293 before and 0.0685 after correction.
The Ratio of minimum to maximum transmission is 0.7470.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       plate
_exptl_crystal_F_000             4638
_exptl_crystal_size_max          0.537
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.079
_refine_diff_density_max         2.269
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2216
_refine_ls_number_reflns         36120
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0468P)^2^+25.2693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27821
_reflns_number_total             36120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03411k2.cif
_cod_data_source_block           mo_d8v3125_0m-1
_cod_database_code               7123716
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.817
_shelx_estimated_absorpt_t_min   0.328
_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(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C138) \\sim Ueq, Uanis(C139) \\sim Ueq, Uanis(C140) \\sim Ueq,
Uanis(C88) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C101)
\\sim Ueq, Uanis(C132) \\sim Ueq, Uanis(C133) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
3. Others
 Sof(H18A)=Sof(C1A)=Sof(H1A)=Sof(C1B)=Sof(H1B)=Sof(C1C)=Sof(H1C)=1-FVAR(1)
 Sof(H188)=Sof(C189)=Sof(H189)=Sof(C190)=Sof(H190)=Sof(C191)=Sof(H191)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C20(H20), C26(H26), C81(H81), C75(H75), C8(H8), C148(H148), C69(H69),
 C14(H14), C166(H166), C2(H2), C160(H160), C142(H142), C32(H32), C136(H136),
 C93(H93), C99(H99), C87(H87), C154(H154)
4.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C25(H25A,H25B), C11(H11A,H11B), C153(H15A,H15B), C23(H23A,
 H23B), C80(H80A,H80B), C79(H79A,H79B), C31(H31A,H31B), C83(H83A,H83B),
 C29(H29A,H29B), C24(H24A,H24B), C21(H21A,H21B), C78(H78A,H78B), C76(H76A,H76B),
  C27(H27A,H27B), C152(H15C,H15D), C28(H28A,H28B), C86(H86A,H86B), C77(H77A,
 H77B), C9(H9A,H9B), C150(H15E,H15F), C149(H14A,H14B), C151(H15G,H15H),
 C10(H10A,H10B), C12(H12A,H12B), C85(H85A,H85B), C13(H13G,H13H), C84(H84A,H84B),
  C30(H30A,H30B), C82(H82A,H82B), C70(H70A,H70B), C73(H73A,H73B), C74(H74A,
 H74B), C71(H71A,H71B), C72(H72A,H72B), C3(H3A,H3B), C171(H17A,H17B), C4(H4A,
 H4B), C161(H16A,H16B), C170(H17C,H17D), C7(H7A,H7B), C6(H6A,H6B), C169(H16C,
 H16D), C167(H16E,H16F), C143(H14C,H14D), C168(H16G,H16H), C5(H5A,H5B),
 C147(H14E,H14F), C155(H15I,H15J), C92(H92A,H92B), C100(H10C,H10D), C95(H95A,
 H95B), C97(H97A,H97B), C98(H98A,H98B), C94(H94A,H94B), C141(H14G,H14H),
 C165(H16I,H16J), C144(H14I,H14J), C162(H16K,H16L), C137(H13A,H13B), C96(H96A,
 H96B), C146(H14K,H14L), C34(H34A,H34B), C19(H19A,H19B), C104(H10E,H10F),
 C37(H37A,H37B), C88(H88A,H88B), C156(H15K,H15L), C158(H15M,H15N), C159(H15O,
 H15P), C101(H10G,H10H), C145(H14M,H14N), C18(H18B,H18C), C90(H90A,H90B),
 C33(H33A,H33B), C91(H91A,H91B), C103(H10I,H10J), C163(H16M,H16N), C35(H35A,
 H35B), C157(H15Q,H15R), C102(H10K,H10L), C138(H13C,H13D), C15(H15S,H15T),
 C89(H89A,H89B), C140(H14O,H14P), C36(H36A,H36B), C139(H13E,H13F), C17(H17E,
 H17F), C164(H16O,H16P), C16(H16Q,H16R)
4.c Aromatic/amide H refined with riding coordinates:
 C174(H174), C199(H199), C41(H41), C105(H105), C57(H57), C182(H182), C40(H40),
 C198(H198), C51(H51), C176(H176), C194(H194), C49(H49), C108(H108), C175(H175),
  C109(H109), C173(H173), C201(H201), C187(H187), C179(H179), C184(H184),
 C60(H60), C107(H107), C200(H200), C39(H39), C42(H42), C53(H53), C56(H56),
 C183(H183), C106(H106), C188(H188), C188(H18A), C55(H55), C172(H172), C50(H50),
  C54(H54), C38(H38), C197(H197), C52(H52), C186(H186), C48(H48), C185(H185),
 C116(H116), C115(H115), C112(H112), C127(H127), C45(H45), C63(H63), C130(H130),
  C118(H118), C117(H117), C120(H120), C119(H119), C64(H64), C124(H124),
 C131(H131), C123(H123), C121(H121), C134(H134), C122(H122), C65(H65), C67(H67),
  C132(H132), C133(H133), C189(H189), C66(H66), C190(H190), C191(H191),
 C1A(H1A), C1B(H1B), C1C(H1C)
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_shelx_res_checksum              26055
_olex2_submission_special_instructions 'No special instructions were received'