Reactions of the spiro monoanion [{(Me2N)Sb(μ-NCy)2}2Sb]− with alcohols and thiols (REH; E = O or S); syntheses of nido-[Sb3(μ-NCy)3(μ3-NCy)(ER)2] anions and the unique antimony(III) imido cubane [(2-NC5H4O)Sb(μ3-NCy)]4 (Cy= cyclohexyl)
Bashall, Alan; Beswick, Michael A.; Feeder, Neil; Hopkins, Alexander D.; Kidd, Sara J.; McPartlin, Mary; Raithby, Paul R.; Wright, Dominic S.; Journal of the Chemical Society, Dalton Transactions  (2000) 1841–; doi:10.1039/b001322f

data_7009473
_publ_section_title
;
 Reactions of the spiro monoanion [{(Me2N)Sb(\m-NCy)2}2Sb]&#x2212; with
 alcohols and thiols (REH; E&#x2005;=&#x2005;O or S); syntheses of
 nido-[Sb3(\m-NCy)3(\m3-NCy)(ER)2] anions and the unique antimony(III)
 imido cubane [(2-NC5H4O)Sb(\m3-NCy)]4 (Cy= cyclohexyl)
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1841
_journal_paper_doi               10.1039/b001322f
_journal_year                    2000
_chemical_formula_sum            'C35.5 H58 Li N8 S2 Sb3'
_chemical_formula_weight         1033.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                70.146(10)
_cell_angle_beta                 87.83(2)
_cell_angle_gamma                89.668(19)
_cell_formula_units_Z            2
_cell_length_a                   11.177(3)
_cell_length_b                   13.746(3)
_cell_length_c                   15.173(4)
_cell_measurement_temperature    223(2)
_cell_volume                     2191.0(10)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker XSCANS'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       theta/2theta
_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  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0939
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7104
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        0.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.965
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_correction_T_min  0.6512
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1030
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.341
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         6004
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0616
_refine_ls_shift/su_max          3.266
_refine_ls_shift/su_mean         0.115
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1013P)^2^+8.7059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1645
_refine_ls_wR_factor_ref         0.2050
_reflns_number_gt                3617
_reflns_number_total             6004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001322f.txt
_cod_data_source_block           nx383
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2191.0(9)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C35.50 H58 Li N8 S2 Sb3'
_cod_database_code               7009473