Functionalization of [Re6Q8(CN)6]4− clusters by methylation of cyanide ligands
Mikhaylov, Maksim A.; Mironova, Alina D.; Brylev, Konstantin A.; Sukhikh, Taisiya S.; Eltsov, Ilia V.; Stass, Dmitri V.; Gushchin, Artem L.; Kitamura, Noboru; Sokolov, Maxim N.; New Journal of Chemistry 43 (2019) 16338–; doi:10.1039/C9NJ02971K

data_7058820
_publ_section_title
;
 Functionalization of [Re6Q8(CN)6]4&#x2212; clusters by methylation of
 cyanide ligands
;
_journal_issue                   41
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16338
_journal_paper_doi               10.1039/C9NJ02971K
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         '2(C6 H9 N3 Re3 Te4), 2(B F4), 3(C3 H7 N O)'
_chemical_formula_sum            'C21 H39 B2 F8 N9 O3 Re6 Te8'
_chemical_formula_weight         2777.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-24 deposited with the CCDC.    2019-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.3530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0153(4)
_cell_length_b                   24.6284(8)
_cell_length_c                   18.1398(5)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.58
_cell_measurement_theta_min      2.39
_cell_volume                     5262.9(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            48414
_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         25.718
_diffrn_reflns_theta_min         1.412
_exptl_absorpt_coefficient_mu    18.153
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.3685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1514 before and 0.0581 after correction. The Ratio of minimum to maximum transmission is 0.4944. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.505
_exptl_crystal_description       plate
_exptl_crystal_F_000             4800
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.378
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         10017
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0250P)^2^+61.7000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7309
_reflns_number_total             10017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02971k2.cif
_cod_data_source_block           amd131_1
_cod_depositor_comments
'Adding full bibliography for 7058819--7058821.cif.'
_cod_database_code               7058820
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.612
_shelx_estimated_absorpt_t_min   0.172
_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. Restrained distances
 O31S-C32S
 1.25 with sigma of 0.02
 N33S-C32S
 1.4 with sigma of 0.02
 N33S-C34S = N33S-C35S
 1.5 with sigma of 0.02
 F13-B4 = F14-B4 = F15-B4 = F16-B4
 1.38 with sigma of 0.002
 F5-B2 = F6-B2 = F7-B2 = F8-B2
 1.38 with sigma of 0.002
 F1-B1 = F3-B1 = F2-B1 = F4-B1 = F11-B3 = F10-B3 = F12-B3 = F9-B3
 1.38 with sigma of 0.002
 C34S-C32S
 2.4 with sigma of 0.04
 C35S-C32S
 2.4 with sigma of 0.04
 F10-F12
 2.28 with sigma of 0.004
 F10-F11
 2.28 with sigma of 0.004
 F10-F9
 2.28 with sigma of 0.004
 F11-F12
 2.28 with sigma of 0.004
 F12-F9
 2.28 with sigma of 0.004
 F11-F9
 2.28 with sigma of 0.004
 F13-F14
 2.28 with sigma of 0.004
 F13-F15
 2.28 with sigma of 0.004
 F13-F16
 2.28 with sigma of 0.004
 F14-F15
 2.28 with sigma of 0.004
 F14-F16
 2.28 with sigma of 0.004
 F15-F16
 2.28 with sigma of 0.004
 F3-F1
 2.28 with sigma of 0.004
 F3-F4
 2.28 with sigma of 0.004
 F3-F2
 2.28 with sigma of 0.004
 F1-F4
 2.28 with sigma of 0.004
 F2-F1
 2.28 with sigma of 0.004
 F4-F2
 2.28 with sigma of 0.004
 F5-F6
 2.28 with sigma of 0.004
 F5-F7
 2.28 with sigma of 0.004
 F5-F8
 2.28 with sigma of 0.004
 F6-F7
 2.28 with sigma of 0.004
 F6-F8
 2.28 with sigma of 0.004
 F7-F8
 2.28 with sigma of 0.004
3. Uiso/Uaniso restraints and constraints
Uiso(C34S) = Uiso(O31S) = Uiso(N33S) = Uiso(C32S) = Uiso(C35S)
Uiso(F13) = Uiso(F14) = Uiso(F15) = Uiso(F16) = Uiso(F9) = Uiso(F10) =
Uiso(F11) = Uiso(F12)
Uiso(F5) = Uiso(F2) = Uiso(F1) = Uiso(F6) = Uiso(F4) = Uiso(F7) = Uiso(F8) =
Uiso(F3)
Uiso(B1) = Uiso(B2)
Uiso(B4) = Uiso(B3)
4. Others
 Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=Sof(B2)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(B1)=FVAR(1)
 Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(B4)=1-FVAR(2)
 Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=Sof(B3)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C12S(H12S), C32S(H32S), C22S(H22S)
5.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C23(H23A,H23B,H23C), C33(H33A,H33B,H33C), C43(H43A,H43B,
 H43C), C53(H53A,H53B,H53C), C63(H63A,H63B,H63C), C14S(H14A,H14B,H14C),
 C15S(H15A,H15B,H15C), C34S(H34A,H34B,H34C), C35S(H35A,H35B,H35C), C24S(H24A,
 H24B,H24C), C25S(H25A,H25B,H25C)
;
_shelx_res_checksum              93731
_olex2_submission_special_instructions 'No special instructions were received'