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_7249446
_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
'C30.2 H42.8 Ag2 F4 N12.2 O4.8 P2 Pt3 S2, 1.5(F6 P), H2 O, 3[C2H3N]'
_chemical_formula_sum            'C36.2 H53.8 Ag2 F13 N15.2 O5.8 P3.5 Pt3 S2'
_chemical_formula_weight         2015.219
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2024-08-09
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2024.07.24 svn.rb972cf6a 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                 112.905(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.235(2)
_cell_length_b                   12.8335(9)
_cell_length_c                   20.6397(18)
_cell_measurement_reflns_used    14965
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.02
_cell_volume                     5913.2(8)
_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    '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 0.9935
_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  0.0547
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.9972
_diffrn_reflns_Laue_measured_fraction_max 0.9935
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            59421
_diffrn_reflns_point_group_measured_fraction_full 0.9972
_diffrn_reflns_point_group_measured_fraction_max 0.9935
_diffrn_reflns_theta_full        25.2425
_diffrn_reflns_theta_max         27.40
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    7.982
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.264
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3796.952
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.012
_refine_diff_density_max         2.3816
_refine_diff_density_min         -2.8646
_refine_diff_density_rms         0.2916
_refine_ls_d_res_high            0.7722
_refine_ls_d_res_low             6.6209
_refine_ls_goodness_of_fit_ref   1.0390
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    77
_refine_ls_number_parameters     660
_refine_ls_number_reflns         13383
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.0367
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.0012
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+101.4778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1283
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              28
_reflns_limit_h_min              -31
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                11853
_reflns_number_total             13383
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ra01671h2.cif
_cod_data_source_block           10-PtC1-PtC1-PtC3-Ag-PF6-MeO-AN-SQ
_cod_database_code               7249446
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H29a,H29b,H29c} of C29, {H22a,H22b,H22c} of C22, {H18a,
  H18b,H18c} of C18, {H13a,H13b,H13c} of C13, {H4a,H4b,H4c} of C4, {H9a,H9b,
  H9c} of C9, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, {H30a,H30b,H30c} of C30, {H1ba,H1bb,H1bc} of C1b, All O(H,
  H) groups
2. Restrained distances
 N13-C1a
 1.14 with sigma of 0.02
 C1a-N13
 1.137 with sigma of 0.01
 C1a-C1b
 1.456 with sigma of 0.01
 C1b-N13
 2.593 with sigma of 0.02
 N13-C1b
 2.59 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N13 \\sim C1a \\sim C1b: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Uanis(C30) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C1b) \\sim Ueq, Uanis(C1a) \\sim Ueq, Uanis(N13) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(F1) = Uanis(F1B) = Uanis(F2) = Uanis(F2B)
Uanis(O2) = Uanis(O2B)
Uanis(N11) = Uanis(N12) = Uanis(C27) = Uanis(C28)
4. Rigid body (RIGU) restrains
 N13, C1a, C1b
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: F1(0.75) F1B(0.25) F2(0.75) F2B(0.25) O2(0.75) O2B(0.25) C1b(0.2)
 H1ba(0.2) H1bb(0.2) H1bc(0.2) N13(0.2) C1a(0.2) O5(0.8) H5(0.8) C30(0.8)
 H30a(0.8) H30b(0.8) H30c(0.8) H1ba(0.2) H1bb(0.2) H1bc(0.2)
6.a Riding coordinates:
 O6(H6b,H6a)
6.b Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C14(H14a,H14b), C23(H23a,H23b), C24(H24a,H24b), C25(H25a,H25b)
6.c Me refined with riding coordinates:
 C4(H4a,H4b,H4c), C9(H9a,H9b,H9c), C13(H13a,H13b,H13c), C18(H18a,H18b,H18c),
 C22(H22a,H22b,H22c), C29(H29a,H29b,H29c), C1b(H1ba,H1bb,H1bc)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C11(H11), C12(H12), C16(H16), C17(H17),
 C20(H20), C27(H27), C28(H28)
6.e Idealised Me refined as rotating group:
 C30(H30a,H30b,H30c)
6.f Idealised tetrahedral OH refined as rotating group:
 O5(H5)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 252 electrons were 
found in a volume of 1141\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3[C2H3N] per Formula Unit which account for 264 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'