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_7249445
_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_absolute_configuration unk
_chemical_formula_moiety         'C28 H39 N8 Pt2 Rh S2, 2(C24 H20 B)'
_chemical_formula_sum            'C79 H85 B2 Cl6 N8 Pt2 Rh S2'
_chemical_formula_weight         1938.166
_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_Hall           'C -2y'
_space_group_name_H-M_alt        'C 1 m 1'
_symmetry_Int_Tables_number      8
_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                 128.641(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.827(4)
_cell_length_b                   25.802(4)
_cell_length_c                   13.476(3)
_cell_measurement_reflns_used    7035
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      3.07
_cell_volume                     4841.6(17)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_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    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      193.35
_diffrn_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 0.9973
_diffrn_measured_fraction_theta_max 0.9970
_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  0.0606
_diffrn_reflns_av_unetI/netI     0.0922
_diffrn_reflns_Laue_measured_fraction_full 0.9973
_diffrn_reflns_Laue_measured_fraction_max 0.9970
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29802
_diffrn_reflns_point_group_measured_fraction_full 0.9941
_diffrn_reflns_point_group_measured_fraction_max 0.9936
_diffrn_reflns_theta_full        25.2425
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    3.298
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1916.104
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_platon_squeeze_details          )
_refine_diff_density_max         1.3418
_refine_diff_density_min         -1.2500
_refine_diff_density_rms         0.1050
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.088(5)
_refine_ls_d_res_high            0.8255
_refine_ls_d_res_low             6.6444
_refine_ls_goodness_of_fit_ref   0.8978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    81
_refine_ls_number_parameters     412
_refine_ls_number_reflns         9154
_refine_ls_number_restraints     365
_refine_ls_restrained_S_all      0.8797
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          -0.0010
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0462P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.990
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              31
_reflns_limit_k_min              -31
_reflns_limit_l_max              16
_reflns_limit_l_min              -16
_reflns_number_gt                8289
_reflns_number_total             9154
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ra01671h2.cif
_cod_data_source_block           5-PtC1-PtC1-RhCpm-BPh4-SQ
_cod_original_cell_volume        4841.6(19)
_cod_original_sg_symbol_Hall     ' C -2y'
_cod_original_formula_sum        'H85 B2 N8 Pt2 Rh1 S2 Cl6 C79'
_cod_database_code               7249445
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H4a,H4b,H4c} of C4, {H9a,H9b,H9c} of C9, All C(H,H) groups
 At 1.5 times of:
  {H16a,H16b,H16c} of C16, {H17a,H17b,H17c} of C17, {H18a,H18b,H18c} of C18,
  {H15a,H15b,H15c} of C15, {H19a,H19b,H19c} of C19
2. Uiso/Uaniso restraints and constraints
Uanis(C10) = Uanis(C11) = Uanis(C12) = Uanis(C13) = Uanis(C14)
Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C19)
3. Rigid body (RIGU) restrains
 C31, C20, C21, C25, B1, C22, C24, C32, C38, C26, C23, C33, C37, C39, C43, C27,
  C34, C36, C40, C42, C28, C30, C35, C41, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, Pt1, C6, C1, S2, S1, N3, N4, N1, N2, Rh1, C5, C7, C8, C9, C2, C3, C4,
 C12, C10, C11, C13, C14, C18, C15, C16, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C10(0.5) C11(0.5) C12(0.5) C13(0.5) C14(0.5) C15(0.5) C16(0.5)
 C17(0.5) C18(0.5) C19(0.5) H15a(0.5) H15b(0.5) H15c(0.5) H16a(0.5) H16b(0.5)
 H16c(0.5) H17a(0.5) H17b(0.5) H17c(0.5) H18a(0.5) H18b(0.5) H18c(0.5)
 H19a(0.5) H19b(0.5) H19c(0.5) H15a(0.5) H15b(0.5) H15c(0.5) H16a(0.5)
 H16b(0.5) H16c(0.5) H17a(0.5) H17b(0.5) H17c(0.5) H18a(0.5) H18b(0.5)
 H18c(0.5) H19a(0.5) H19b(0.5) H19c(0.5) H15a(0.5) H15b(0.5) H15c(0.5)
 H16a(0.5) H16b(0.5) H16c(0.5) H18a(0.5) H18b(0.5) H18c(0.5) H19a(0.5)
 H19b(0.5) H19c(0.5) H17a(0.5) H17b(0.5) H17c(0.5) H15a(0.5) H15b(0.5)
 H15c(0.5) H16a(0.5) H16b(0.5) H16c(0.5) H17a(0.5) H17b(0.5) H17c(0.5)
 H18a(0.5) H18b(0.5) H18c(0.5) H19a(0.5) H19b(0.5) H19c(0.5) H15a(0.5)
 H15b(0.5) H15c(0.5) H16a(0.5) H16b(0.5) H16c(0.5) H18a(0.5) H18b(0.5)
 H18c(0.5) H19a(0.5) H19b(0.5) H19c(0.5) H15a(0.5) H15b(0.5) H15c(0.5)
 H16a(0.5) H16b(0.5) H16c(0.5) H17a(0.5) H17b(0.5) H17c(0.5) H18a(0.5)
 H18b(0.5) H18c(0.5) H19a(0.5) H19b(0.5) H19c(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b)
5.b Me refined with riding coordinates:
 C4(H4a,H4b,H4c), C9(H9a,H9b,H9c), C15(H15a,H15b,H15c), C16(H16a,H16b,H16c),
 C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), C19(H19a,H19b,H19c)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C21(H21), C22(H22), C23(H23), C24(H24),
 C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34),
  C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'