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_7058821
_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         'C12 H18 N6 Re6 S8, 2(C F3 O3 S), 2(C2 H3 N)'
_chemical_formula_sum            'C18 H24 F6 N8 O6 Re6 S10'
_chemical_formula_weight         2000.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-05-24 deposited with the CCDC.    2019-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.8829(13)
_cell_length_b                   11.7447(7)
_cell_length_c                   16.8444(9)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.71
_cell_measurement_theta_min      2.49
_cell_volume                     4527.0(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0568
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            48639
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.780
_exptl_absorpt_coefficient_mu    16.506
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.2444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1515 before and 0.0670 after correction. The Ratio of minimum to maximum transmission is 0.3277. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.935
_exptl_crystal_description       prism
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.932
_refine_diff_density_min         -2.301
_refine_diff_density_rms         0.359
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.241
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.241
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0160P)^2^+435.4167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1653
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3327
_reflns_number_total             3987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02971k2.cif
_cod_data_source_block           amd411_1
_cod_depositor_comments
'Adding full bibliography for 7058819--7058821.cif.'
_cod_database_code               7058821
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.352
_shelx_estimated_absorpt_t_min   0.069
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Free rotating group:
 N1S(C2S,C3S)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C23(H23A,H23B,H23C), C33(H33A,H33B,H33C), C3S(H3SA,H3SB,
 H3SC)
;
_shelx_res_checksum              50343
_olex2_submission_special_instructions 'No special instructions were received'