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_7058819
_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 Se4), 2(B F4), 0.5(O2 H4), 3(C2 H3 N)'
_chemical_formula_sum            'C18 H29 B2 F8 N9 O Re6 Se8'
_chemical_formula_weight         2309.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-02-18
_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                 96.5236(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9966(11)
_cell_length_b                   23.4741(15)
_cell_length_c                   11.6818(6)
_cell_measurement_reflns_used    5419
_cell_measurement_temperature    155.15
_cell_measurement_theta_max      29.78
_cell_measurement_theta_min      2.41
_cell_volume                     4630.6(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      155.15
_diffrn_measured_fraction_theta_full 0.999
_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  0.0486
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            26281
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.206
_exptl_absorpt_coefficient_mu    21.970
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1195 before and 0.0515 after correction. The Ratio of minimum to maximum transmission is 0.4715. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.306
_exptl_crystal_description       needle
_exptl_crystal_F_000             4028
_exptl_crystal_size_max          0.412
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.056
_refine_diff_density_max         2.352
_refine_diff_density_min         -2.499
_refine_diff_density_rms         0.353
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         8783
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0353P)^2^+94.9328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6526
_reflns_number_total             8783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02971k2.cif
_cod_data_source_block           amd74_2
_cod_depositor_comments
'Adding full bibliography for 7058819--7058821.cif.'
_cod_database_code               7058819
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F8-B2 = F5-B2 = F7-B2 = F6-B2
 1.3 with sigma of 0.02
 C4S-C5S
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C4 \\sim N4: within 1.7A with sigma of 0.008 and sigma for terminal atoms of
0.016
C2 \\sim N2: within 1.7A with sigma of 0.008 and sigma for terminal atoms of
0.016
C11 \\sim N1: within 1.7A with sigma of 0.008 and sigma for terminal atoms of
0.016
C6 \\sim N6: within 1.7A with sigma of 0.008 and sigma for terminal atoms of
0.016
Uiso(O1S) = Uiso(O2S)
4. Others
 Fixed Sof: O1S(0.5) O2S(0.5)
5.a Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C21(H21A,H21B,H21C), C31(H31A,H31B,H31C), C41(H41A,H41B,
 H41C), C51(H51A,H51B,H51C), C61(H61A,H61B,H61C), C1S(H1SA,H1SB,H1SC), C7S(H7SA,
 H7SB,H7SC)
;
_shelx_res_checksum              32721
_olex2_submission_special_instructions 'No special instructions were received'