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_7248260
_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 Mo3 N6 Re3 S8'
_chemical_formula_sum            'C42 H54 Mo3 N6 Re3 S8'
_chemical_formula_weight         1745.81
_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                   14.2677(11)
_cell_length_b                   14.2677(11)
_cell_length_c                   24.473(4)
_cell_measurement_reflns_used    4657
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.50
_cell_measurement_theta_min      2.62
_cell_volume                     4981.9(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_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_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16324
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.569
_diffrn_reflns_theta_min         2.617
_exptl_absorpt_coefficient_mu    8.366
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0675 before and 0.0537 after correction.
The Ratio of minimum to maximum transmission is 0.8244.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.328
_exptl_crystal_description       plate
_exptl_crystal_F_000             3308
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3483
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0245
_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^)+(0.0090P)^2^+1.4157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2378
_reflns_number_total             3483
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01229h2.cif
_cod_data_source_block           lap737
_cod_depositor_comments
'Adding full bibliography for 7248256--7248264.cif.'
_cod_original_cell_volume        4981.8(10)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7248260
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.634
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Re1, Mo1}
{Re2, Mo2}
3. Restrained distances
 C17A-C16 = C17-C16 = C24-C23 = C25-C24
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq, Uanis(C17A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Re1) = Uanis(Mo1)
Uanis(Re2) = Uanis(Mo2)
5. Others
 1*[Sof(Re1)+Sof(Mo1)]+0.5*[Sof(Re2)+Sof(Mo2)]=0.75 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)
 Sof(H16C)=Sof(H16D)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(3)
 Sof(H16A)=Sof(H16B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=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)
6.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C16(H16C,H16D), C24(H24A,H24B)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C14(H14), C15(H15), C21(H21), C22(H22)
6.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              99744
_olex2_submission_special_instructions 'No special instructions were received'