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_7248259
_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         'C30 H30 Mo2.652 N6 Re3.348 S8'
_chemical_formula_sum            'C30 H30 Mo2.65 N6 Re3.35 S8'
_chemical_formula_weight         1609.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-24 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                114.4320(10)
_cell_angle_beta                 90.7490(10)
_cell_angle_gamma                109.1920(10)
_cell_formula_units_Z            1
_cell_length_a                   9.3458(4)
_cell_length_b                   10.5903(4)
_cell_length_c                   11.8441(5)
_cell_measurement_reflns_used    5643
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.23
_cell_volume                     992.72(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10546
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.388
_diffrn_reflns_theta_min         1.918
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    11.436
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1144 before and 0.0346 after correction. The Ratio of minimum to maximum transmission is 0.6360. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.692
_exptl_crystal_description       prism
_exptl_crystal_F_000             743
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         4061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0159P)^2^+0.0200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0402
_refine_ls_wR_factor_ref         0.0418
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3615
_reflns_number_total             4061
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01229h2.cif
_cod_data_source_block           lap258
_cod_depositor_comments
'Adding full bibliography for 7248256--7248264.cif.'
_cod_database_code               7248259
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.394
_shelx_estimated_absorpt_t_min   0.233
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{Re1, Mo1}
{Re2, Mo2}
{Re3, Mo3}
3. Uiso/Uaniso restraints and constraints
Uanis(Re1) = Uanis(Mo1)
Uanis(Re2) = Uanis(Mo2)
Uanis(Re3) = Uanis(Mo3)
4. Others
 Sof(Mo1)=1-FVAR(1)
 Sof(Re1)=FVAR(1)
 Sof(Mo2)=1-FVAR(2)
 Sof(Re2)=FVAR(2)
 Sof(Mo3)=1-FVAR(3)
 Sof(Re3)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C21(H21), C22(H22),
 C23(H23), C24(H24), C25(H25), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35)
;
_shelx_res_checksum              10675
_olex2_submission_special_instructions 'No special instructions were received'