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

data_7123715
_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, 2(C H2 Cl2)'
_chemical_formula_sum            'C69 H92 Cl8 Cr N O4 P2 Pt Ru'
_chemical_formula_weight         1693.13
_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             2017-08-09
_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                86.8201(13)
_cell_angle_beta                 88.6083(13)
_cell_angle_gamma                73.9461(12)
_cell_formula_units_Z            2
_cell_length_a                   13.8990(5)
_cell_length_b                   14.2368(5)
_cell_length_c                   18.9706(7)
_cell_measurement_reflns_used    9679
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.412
_cell_measurement_theta_min      2.612
_cell_volume                     3601.7(2)
_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 0.999
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            95397
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.408
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.680
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0674 before and 0.0499 after correction.
The Ratio of minimum to maximum transmission is 0.8970.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       prism
_exptl_crystal_F_000             1714
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         14720
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+4.2486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0447
_refine_ls_wR_factor_ref         0.0465
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13553
_reflns_number_total             14720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03411k2.cif
_cod_data_source_block           mo_d8v3035_0m-morten
_cod_database_code               7123715
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.696
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 Cl6-C69 \\sim Cl5A-C69 \\sim Cl5-C69 \\sim Cl6A-C69
 with sigma of 0.01
3. Others
 Sof(H69C)=Sof(H69D)=Sof(Cl6A)=Sof(Cl5A)=1-FVAR(1)
 Sof(Cl5)=Sof(Cl6)=Sof(H69A)=Sof(H69B)=FVAR(1)
 Sof(H37C)=Sof(H37D)=Sof(H34C)=Sof(H34D)=Sof(H32A)=Sof(H35C)=Sof(H35D)=
 Sof(C33A)=Sof(H33C)=Sof(H33D)=Sof(C36A)=Sof(H36C)=Sof(H36D)=1-FVAR(2)
 Sof(H37A)=Sof(H37B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H34A)=Sof(H34B)=Sof(C36)=
 Sof(H36A)=Sof(H36B)=Sof(H32)=Sof(H35A)=Sof(H35B)=FVAR(2)
 Sof(C68A)=Sof(H68C)=Sof(H68D)=Sof(Cl8A)=1-FVAR(3)
 Sof(Cl8)=Sof(C68)=Sof(H68A)=Sof(H68B)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C8(H8), C14(H14), C26(H26), C2(H2), C20(H20), C32(H32), C32(H32A)
4.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C37(H37C,H37D), C15(H15A,H15B), C3(H3A,H3B), C25(H25A,H25B),
 C6(H6A,H6B), C18(H18A,H18B), C17(H17A,H17B), C19(H19A,H19B), C31(H31A,H31B),
 C12(H12A,H12B), C28(H28A,H28B), C22(H22A,H22B), C23(H23A,H23B), C33(H33A,H33B),
  C7(H7A,H7B), C5(H5A,H5B), C16(H16A,H16B), C27(H27A,H27B), C30(H30A,H30B),
 C11(H11A,H11B), C10(H10A,H10B), C34(H34A,H34B), C34(H34C,H34D), C24(H24A,H24B),
  C29(H29A,H29B), C9(H9A,H9B), C4(H4A,H4B), C36(H36A,H36B), C13(H13A,H13B),
 C21(H21A,H21B), C35(H35A,H35B), C35(H35C,H35D), C68(H68A,H68B), C69(H69A,H69B),
  C69(H69C,H69D), C33A(H33C,H33D), C36A(H36C,H36D), C68A(H68C,H68D)
4.c Aromatic/amide H refined with riding coordinates:
 C38(H38), C56(H56), C64(H64), C48(H48), C49(H49), C51(H51), C65(H65),
 C63(H63), C55(H55), C50(H50), C60(H60), C42(H42), C39(H39), C67(H67), C57(H57),
  C66(H66), C41(H41), C53(H53), C45(H45), C40(H40), C52(H52), C54(H54)
;
_shelx_res_checksum              42991
_olex2_submission_special_instructions 'No special instructions were received'