Molecular heterometallic clusters [Re6−xMoxS8L6] (x = 2–3, L = py, etpy, tbp): negligible influence of the x value on the crystal structures
Lappi, Tatiana I.; Gaifulin, Yakov M.; Sukhikh, Taisiya S.; Gaifulina, Viktoria K.; Yanshole, Vadim V.; Cordier, Stephane; Naumov, Nikolay G.; CrystEngComm 26 (2024) 1720–1729; doi:10.1039/D3CE01229H

data_7248256
_publ_section_title
;
 Molecular heterometallic clusters [Re6&#x2212;xMoxS8L6] (x = 2--3, L =
 py, etpy, tbp): negligible influence of the x value on the crystal
 structures
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              1720
_journal_page_last               1729
_journal_paper_doi               10.1039/D3CE01229H
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C42 H54 Mo2.7 N6 Re3.3 S8'
_chemical_formula_sum            'C42 H54 Mo2.7 N6 Re3.3 S8'
_chemical_formula_weight         1772.89
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-11-24 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2868(2)
_cell_length_b                   14.2868(2)
_cell_length_c                   24.4236(8)
_cell_measurement_reflns_used    3143
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.68
_cell_measurement_theta_min      2.62
_cell_volume                     4985.17(19)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.982
_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  0.0170
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            6112
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.651
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.012
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0494 before and 0.0331 after correction. The Ratio of minimum to maximum transmission is 0.8388. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.362
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             3348
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3043
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0189
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0023P)^2^+10.4881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0363
_refine_ls_wR_factor_ref         0.0390
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2304
_reflns_number_total             3043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01229h2.cif
_cod_data_source_block           lap160
_cod_depositor_comments
'Adding full bibliography for 7248256--7248264.cif.'
_cod_original_cell_volume        4985.2(2)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C42 H54 Mo2.70 N6 Re3.30 S8'
_cod_database_code               7248256
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.253
_shelx_estimated_absorpt_t_min   0.187
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Re2, Mo2}
{Re1, Mo1}
3. Uiso/Uaniso restraints and constraints
Uanis(Re1) = Uanis(Mo1)
Uanis(Re2) = Uanis(Mo2)
4. Others
 1*[Sof(Re1)+Sof(Mo1)]+0.5*[Sof(Re2)+Sof(Mo2)]=0.825 with esd of 0.0001
 Sof(Mo1)=1-FVAR(1)
 Sof(Re1)=FVAR(1)
 Sof(Mo2)=0.5*(1-FVAR(3))
 Sof(Re2)=0.5*FVAR(3)
 Fixed Sof: C24(0.5) H24A(0.5) H24B(0.5) C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C24(H24A,H24B)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C14(H14), C15(H15), C21(H21), C22(H22)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              48166
_olex2_submission_special_instructions 'No special instructions were received'