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_7249442
_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.
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_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
'C26 H36 N8 Pt2 Rh S2, F6 P, 2[C2H3N], 1[C2H3N]'
_chemical_formula_sum            'C32 H45 F6 N11 P Pt2 Rh S2'
_chemical_formula_weight         1285.946
_space_group_crystal_system      tetragonal
_space_group_IT_number           80
_space_group_name_Hall           'I 4bw'
_space_group_name_H-M_alt        'I 41'
_symmetry_Int_Tables_number      80
_audit_creation_date             2024-01-22
_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                90
_cell_formula_units_Z            4
_cell_length_a                   12.3687(11)
_cell_length_b                   12.3687(11)
_cell_length_c                   27.8127(18)
_cell_measurement_reflns_used    5534
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.29
_cell_volume                     4254.9(6)
_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    SIR97
_diffrn_ambient_temperature      193.35
_diffrn_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 0.9969
_diffrn_measured_fraction_theta_max 0.9976
_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  0.0534
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_Laue_measured_fraction_full 0.9969
_diffrn_reflns_Laue_measured_fraction_max 0.9976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            21520
_diffrn_reflns_point_group_measured_fraction_full 0.9958
_diffrn_reflns_point_group_measured_fraction_max 0.9963
_diffrn_reflns_theta_full        25.2425
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    7.141
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.007
_exptl_crystal_description       prism
_exptl_crystal_F_000             2452.888
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.8008
_refine_diff_density_min         -2.2187
_refine_diff_density_rms         0.2241
_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   0.042(6)
_refine_ls_d_res_high            0.7699
_refine_ls_d_res_low             6.1843
_refine_ls_goodness_of_fit_ref   1.0062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    39
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4875
_refine_ls_number_restraints     290
_refine_ls_restrained_S_all      0.9761
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+8.2668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.995
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              35
_reflns_limit_l_min              -36
_reflns_number_gt                4121
_reflns_number_total             4875
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ra01671h2.cif
_cod_data_source_block           6-Pt2-C1-RhCod-PF6-I41-SQ
_cod_original_sg_symbol_Hall     ' I 4bw'
_cod_original_formula_sum        'C32 H45 F6 N11 P1 Pt2 Rh1 S2'
_cod_database_code               7249442
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups
2. Restrained distances
 C10-C11
 1.37 with sigma of 0.02
 C10-C17 = C13-C14
 1.5 with sigma of 0.02
 C11-C12
 1.52 with sigma of 0.02
 C12-C13
 1.54 with sigma of 0.02
 C14-C15
 1.36 with sigma of 0.02
 C15-C16
 1.51 with sigma of 0.02
 C16-C17
 1.53 with sigma of 0.02
 C10-C12
 2.58 with sigma of 0.04
 C10-C16 = C15-C17
 2.54 with sigma of 0.04
 C11-C13 = C12-C14
 2.55 with sigma of 0.04
 C13-C15 = C14-C16
 2.56 with sigma of 0.04
 C11-C10 \\sim C15-C14
 with sigma of 0.02
 C17-C10 \\sim C12-C11 \\sim C16-C15 \\sim C14-C13 \\sim C17-C16 \\sim C12-C13
 with sigma of 0.02
 C10-C12 \\sim C10-C16 \\sim C11-C13 \\sim C11-C17 \\sim C12-C14 \\sim C13-C15
\\sim C14-C16 \\sim C15-C17
 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C14) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 P1, F3, F3, F1, F1, F5, F5, F2, F2, F4, F4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C10, C11, C12, C13, C14, C15, C16, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, N1, C2, C5, N2, C3, N3, C4, C6, C7, N4, C8, C9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: F2(0.5) F3(0.5) F4(0.5) F5(0.5) C10(0.5) C11(0.5) C12(0.5)
 C13(0.5) C14(0.5) C15(0.5) C16(0.5) C17(0.5) C1a(0.5) C19(0.5) H1aa(0.5)
 H1ab(0.5) H1ac(0.5) N5(0.5) H17a(0.5) H17b(0.5) H11(0.5) H14(0.5) H15(0.5)
 H10(0.5) H12a(0.5) H12b(0.5) H13a(0.5) H13b(0.5) H16a(0.5) H16b(0.5)
 Fixed Uiso: C18(0.125883) N19(0.125717) C20(0.1259) C23(0.08) C21(0.08)
 N5(0.016421) C19(0.089446) C1a(0.089441)
6.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C15(H15), C10(H10)
6.b Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C17(H17a,H17b), C12(H12a,H12b), C13(H13a,H13b), C16(H16a,H16b)
6.c Me refined with riding coordinates:
 C4(H4a,H4b,H4c), C9(H9a,H9b,H9c)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 248 electrons were 
found in a volume of 1356\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 2[C2H3N], 1[C2H3N] per Formula Unit 
which account for 264 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.0
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'