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_7248261
_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         'C54 H78 Mo2.7 N6 Re3.3 S8'
_chemical_formula_sum            'C54 H78 Mo2.7 N6 Re3.3 S8'
_chemical_formula_weight         1941.20
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :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                   26.7541(6)
_cell_length_b                   26.7541(6)
_cell_length_c                   9.3946(3)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.64
_cell_measurement_theta_min      2.42
_cell_volume                     6724.5(3)
_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      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0613
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            54716
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.701
_diffrn_reflns_theta_min         0.761
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.690
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1007 before and 0.0611 after correction. The Ratio of minimum to maximum transmission is 0.6623. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_description       needle
_exptl_crystal_F_000             3732
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.195
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6401
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0125P)^2^+29.8941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5616
_reflns_number_total             6401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01229h2.cif
_cod_data_source_block           gy1144
_cod_depositor_comments
'Adding full bibliography for 7248256--7248264.cif.'
_cod_original_cell_volume        6724.5(4)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_original_formula_sum        'C54 H78 Mo2.70 N6 Re3.30 S8'
_cod_database_code               7248261
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.652
_shelx_estimated_absorpt_t_min   0.286
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7967(6)
 0.2033(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Shared sites
{Re1, Mo1}
{Re2, Mo2}
{Re3, Mo3}
4. Restrained distances
 C26-C272 \\sim C26-C281 \\sim C26-C282 \\sim C26-C291 \\sim C26-C292 \\sim
C26-C271
 with sigma of 0.02
 C36-C381 \\sim C36-C372 \\sim C371-C36 \\sim C392-C36 \\sim C391-C36 \\sim
C382-C36
 with sigma of 0.02
5. Rigid bond restraints
 C26, C272, C282, C292
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C271, C281, C291
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C36, C371, C381, C391
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C36, C372, C382, C392
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
6. Uiso/Uaniso restraints and constraints
C26 \\sim C272 \\sim C282 \\sim C292: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C26 \\sim C271 \\sim C281 \\sim C291: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C36 \\sim C371 \\sim C381 \\sim C391: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C36 \\sim C372 \\sim C382 \\sim C392: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.7A
Uanis(Re1) = Uanis(Mo1)
Uanis(Re2) = Uanis(Mo2)
Uanis(Re3) = Uanis(Mo3)
7. Others
 1*[Sof(Re1)+Sof(Mo1)]+1*[Sof(Re2)+Sof(Mo2)]+1*[Sof(Re3)+Sof(Mo3)]=1.65 with
 esd of 0.0001
 Sof(C272)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C282)=Sof(H28D)=Sof(H28E)=
 Sof(H28F)=Sof(C292)=Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(1)
 Sof(C271)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C281)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=Sof(C291)=Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(1)
 Sof(C372)=Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C382)=Sof(H38D)=Sof(H38E)=
 Sof(H38F)=Sof(C392)=Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(2)
 Sof(C371)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C381)=Sof(H38A)=Sof(H38B)=
 Sof(H38C)=Sof(C391)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(2)
 Sof(Mo1)=1-FVAR(3)
 Sof(Re1)=FVAR(3)
 Sof(Mo2)=1-FVAR(4)
 Sof(Re2)=FVAR(4)
 Sof(Mo3)=1-FVAR(5)
 Sof(Re3)=FVAR(5)
8.a Me refined with riding coordinates:
 C271(H27A,H27B,H27C), C281(H28A,H28B,H28C), C291(H29A,H29B,H29C), C272(H27D,
 H27E,H27F), C282(H28D,H28E,H28F), C292(H29D,H29E,H29F)
8.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C14(H14), C15(H15), C21(H21), C22(H22), C24(H24),
 C25(H25), C31(H31), C32(H32), C34(H34), C35(H35)
8.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C371(H37A,H37B,
 H37C), C381(H38A,H38B,H38C), C391(H39A,H39B,H39C), C372(H37D,H37E,H37F),
 C382(H38D,H38E,H38F), C392(H39D,H39E,H39F)
;
_shelx_res_checksum              67276
_olex2_submission_special_instructions 'No special instructions were received'