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_7248262
_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         '2(C27 H39 Mo1.5 N3 Re1.5 S4), 2.584(C2 H3 N)'
_chemical_formula_sum            'C59.17 H85.75 Mo3 N8.59 Re3 S8'
_chemical_formula_weight         2020.18
_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             2023-07-19
_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                105.271(3)
_cell_angle_beta                 103.906(3)
_cell_angle_gamma                100.383(3)
_cell_formula_units_Z            2
_cell_length_a                   14.3459(11)
_cell_length_b                   15.5318(13)
_cell_length_c                   18.3357(14)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      2.32
_cell_volume                     3694.1(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0541
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            61226
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.610
_diffrn_reflns_theta_min         1.514
_exptl_absorpt_coefficient_mu    5.655
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0998 before and 0.0542 after correction.
The Ratio of minimum to maximum transmission is 0.7669.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_description       needle
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         20697
_refine_ls_number_restraints     172
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0316P)^2^+1.6229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14973
_reflns_number_total             20697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01229h2.cif
_cod_data_source_block           lap738
_cod_depositor_comments
'Adding full bibliography for 7248256--7248264.cif.'
_cod_database_code               7248262
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.505
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Re1, Mo1}
{Re2, Mo2}
{Re3, Mo3}
{Re4, Mo4}
{Re5, Mo5}
{Re6, Mo6}
3. Restrained distances
 C16A-C15 = C16-C15 = C17-C15 = C17A-C15 = C18-C15 = C18A-C15
 1.54 with sigma of 0.02
 C5-C6
 1.456 with sigma of 0.01
 C1-C2
 1.456 with sigma of 0.01
 C3-N7
 1.137 with sigma of 0.01
 C6-N9
 2.593 with sigma of 0.02
 C2-N8
 2.593 with sigma of 0.02
 C3-C4
 1.456 with sigma of 0.01
 C4-N7
 2.593 with sigma of 0.02
 C67A-C65 = C67-C65 = C66A-C65 = C66-C65 = C68A-C65 = C68-C65
 1.54 with sigma of 0.02
 C1-N8
 1.137 with sigma of 0.01
 C56A-C55 = C56-C55 = C58A-C55 = C58-C55 = C57A-C55 = C57-C55
 1.54 with sigma of 0.02
 C5-N9
 1.137 with sigma of 0.01
 C67-C68 \\sim C68-C66 \\sim C66-C67
 with sigma of 0.02
 C67A-C68A \\sim C68A-C66A \\sim C66A-C67A
 with sigma of 0.02
 C56A-C57A \\sim C57A-C58A \\sim C56A-C58A
 with sigma of 0.02
 C57-C56 \\sim C56-C58 \\sim C57-C58
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N9 \\sim C5 \\sim C6: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
N8 \\sim C1 \\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
N7 \\sim C3 \\sim C4: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uiso(C1) = Uiso(N8) = Uiso(C2) = Uiso(C4) = Uiso(N7) = Uiso(C3) = Uiso(C6) =
Uiso(N9) = Uiso(C5)
Uanis(Re1) = Uanis(Mo1)
Uanis(Re2) = Uanis(Mo2)
Uanis(Re3) = Uanis(Mo3)
Uanis(Re4) = Uanis(Mo4)
Uanis(Re5) = Uanis(Mo5)
Uanis(Re6) = Uanis(Mo6)
5. Rigid body (RIGU) restrains
 C65, C66, C67, C68
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N9, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N8, C1, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C65, C66A, C68A, C67A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N7, C3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C55, C56A, C57A, C58A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C55, C56, C57, C58
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15, C17A, C18A, C16A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(Re1)+Sof(Mo1)]+1*[Sof(Re2)+Sof(Mo2)]+1*[Sof(Re3)+Sof(Mo3)]+1*[Sof(Re4)+
 Sof(Mo4)]+1*[Sof(Re5)+Sof(Mo5)]+1*[Sof(Re6)+Sof(Mo6)]=3 with esd of 0.0001
 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)
 Sof(Mo4)=1-FVAR(4)
 Sof(Re4)=FVAR(4)
 Sof(Mo5)=1-FVAR(5)
 Sof(Re5)=FVAR(5)
 Sof(Mo6)=1-FVAR(6)
 Sof(Re6)=FVAR(6)
 Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18A)=Sof(H18D)=Sof(H18E)=
 Sof(H18F)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(7)
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(7)
 Sof(C56A)=Sof(H56D)=Sof(H56E)=Sof(H56F)=Sof(C57A)=Sof(H57D)=Sof(H57E)=
 Sof(H57F)=Sof(C58A)=Sof(H58D)=Sof(H58E)=Sof(H58F)=1-FVAR(8)
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=
 Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=FVAR(8)
 Sof(C66A)=Sof(H66D)=Sof(H66E)=Sof(H66F)=Sof(C68A)=Sof(H68D)=Sof(H68E)=
 Sof(H68F)=Sof(C67A)=Sof(H67D)=Sof(H67E)=Sof(H67F)=Sof(N8)=Sof(C1)=Sof(C2)=
 Sof(H2A)=Sof(H2B)=Sof(H2C)=1-FVAR(9)
 Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(N7)=Sof(C3)=Sof(C4)=Sof(H4A)=
 Sof(H4B)=Sof(H4C)=Sof(N9)=Sof(C5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=FVAR(9)
7.a Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C66(H66A,H66B,H66C), C67(H67A,
 H67B,H67C), C68(H68A,H68B,H68C), C17A(H17D,H17E,H17F), C18A(H18D,H18E,H18F),
 C16A(H16D,H16E,H16F), C56A(H56D,H56E,H56F), C57A(H57D,H57E,H57F), C58A(H58D,
 H58E,H58F), C66A(H66D,H66E,H66F), C68A(H68D,H68E,H68F), C67A(H67D,H67E,H67F)
7.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C13(H13), C14(H14), C20(H20), C21(H21), C23(H23),
 C24(H24), C30(H30), C31(H31), C33(H33), C34(H34), C40(H40), C41(H41), C43(H43),
  C44(H44), C50(H50), C51(H51), C53(H53), C54(H54), C60(H60), C61(H61),
 C63(H63), C64(H64)
7.c Idealised Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C6(H6A,H6B,H6C)
7.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C3A(H3AA,H3AB,H3AC), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              68136
_olex2_submission_special_instructions 'No special instructions were received'