Restriction of reaction sites on metal-sulfide cores induced by steric repulsion of bis-N-heterocyclic carbene ligands in trinuclear complexes bearing triply bridging sulfide ligands.
Yabune, Natsuki; Nakajima, Hiroshi; Nishioka, Takanori; RSC advances 14 (2024) 29355–29367; doi:10.1039/d4ra01671h

data_7249444
_publ_section_title
;
 Restriction of reaction sites on metal-sulfide cores induced by steric
 repulsion of bis-N-heterocyclic carbene ligands in trinuclear complexes
 bearing triply bridging sulfide ligands.
;
_journal_issue                   40
_journal_name_full               'RSC advances'
_journal_page_first              29355
_journal_page_last               29367
_journal_paper_doi               10.1039/d4ra01671h
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C33 H48 N12 Pt3 S2, 2(F6 P), 1.5(C4 H6 N2)'
_chemical_formula_sum            'C39 H57 F12 N15 P2 Pt3 S2'
_chemical_formula_weight         1675.282
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_Int_Tables_number      176
_audit_creation_date             2024-01-19
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2024.01.11 svn.r2f8d729c for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2024-08-14 deposited with the CCDC.	2024-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.1996(6)
_cell_length_b                   14.1996(6)
_cell_length_c                   16.3484(7)
_cell_measurement_reflns_used    8359
_cell_measurement_temperature    193
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.13
_cell_volume                     2854.7(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193.35
_diffrn_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 0.9972
_diffrn_measured_fraction_theta_max 0.9978
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 0.9972
_diffrn_reflns_Laue_measured_fraction_max 0.9978
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29775
_diffrn_reflns_point_group_measured_fraction_full 0.9972
_diffrn_reflns_point_group_measured_fraction_max 0.9978
_diffrn_reflns_theta_full        25.2425
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    7.542
_exptl_absorpt_correction_T_max  0.444
_exptl_absorpt_correction_T_min  0.270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.949
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1594.866
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.108
_refine_diff_density_max         2.3369
_refine_diff_density_min         -1.1224
_refine_diff_density_rms         0.1371
_refine_ls_d_res_high            0.7698
_refine_ls_d_res_low             6.5122
_refine_ls_goodness_of_fit_ref   1.0282
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    4
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2264
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0282
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          -0.0006
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+16.0038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                2259
_reflns_number_total             2264
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ra01671h2.cif
_cod_data_source_block           Pt-C3-Me-PF6-acetonitrile
_cod_database_code               7249444
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H8a(0.5) H8b(0.5) H8c(0.5)
 Fixed Uiso: H2(0.06303) H3(0.06148) H4a(0.07088) H4b(0.07088) H4c(0.07088)
 H5a(0.0602) H5b(0.0602) H6a(0.06208) H6b(0.06208)
 Fixed X: H2(0.35905) H3(0.40879) H4a(0.23467) H4b(0.28696) H4c(0.36397)
 H5a(0.11385) H5b(0.19334) H6a(0.22334) H6b(0.3172)
 Fixed Y: H2(0.44526) H3(0.3058) H4a(0.05533) H4b(0.08369) H4c(0.12308)
 H5a(0.3334) H5b(0.43785) H6a(0.51467) H6b(0.48378)
 Fixed Z: H2(0.05969) H3(0.03006) H4a(0.08506) H4b(0.17468) H4c(0.09577)
 H5a(0.18178) H5b(0.12882) H6a(0.25) H6b(0.25)
3.a Everything fixed:
 H2, H3, H4a, H4b, H4c, H5a, H5b, H6a, H6b
3.b Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c)
;
_olex2_submission_special_instructions 'No special instructions were received'