First oxido-bridged cubo-octahedral hexanuclear rhenium clusters.
Krawczyk, Marta S.; Krawczyk, Monika K.; Siczek, Miłosz; Lis, Tadeusz; Inorganic chemistry 53 (2014) 6578–6584; doi:10.1021/ic500162x

data_4338830
_publ_section_title
;
 First oxido-bridged cubo-octahedral hexanuclear rhenium clusters.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6578
_journal_page_last               6584
_journal_paper_doi               10.1021/ic500162x
_journal_volume                  53
_journal_year                    2014
_chemical_formula_iupac
'[Re6 O12 (C5 H5 N)6] + B (C6 H6)4 - 2(CH3CN)'
_chemical_formula_moiety         'C36 H42 N6 O12 Re6, C24 H20 B, 2(C2 H3 N)'
_chemical_formula_sum            'C64 H68 B N8 O12 Re6'
_chemical_formula_weight         2269.27
_chemical_name_systematic
; 
Dodeca-\m-oxido-hexa(3-methylpyridine)-octahedro-hexarenium(12 Re-Re)(1+)
-acetonitrile (1/2) tetraphenylborate  
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.45(3)
_cell_angle_beta                 78.09(3)
_cell_angle_gamma                79.70(3)
_cell_formula_units_Z            2
_cell_length_a                   10.475(3)
_cell_length_b                   18.116(6)
_cell_length_c                   18.230(6)
_cell_measurement_reflns_used    4843
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.75
_cell_measurement_theta_min      2.71
_cell_volume                     3271.4(19)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.35.19'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.35.19'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.35.19'
_computing_molecular_graphics    'XP in SHELXTL (Bruker, 1997)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 2013), publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_device_type  'Xcalibur with CCD Ruby detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_sigmaI/netI    0.1302
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24939
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.82
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    11.123
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_correction_T_min  0.233
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2118
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.06
_refine_diff_density_min         -1.82
_refine_diff_density_rms         0.296
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         14684
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0140P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                8484
_reflns_number_total             14684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500162x_si_003.cif
_cod_data_source_block           marta43a
_cod_depositor_comments
'Adding full bibliography for 4338829--4338832.cif.'
_cod_original_cell_volume        3271.4(18)
_cod_database_code               4338830