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_7009474
_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            'C47.5 H66 N8 O4 Sb4'
_chemical_formula_weight         1300.08
_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                65.45(3)
_cell_angle_beta                 74.73(3)
_cell_angle_gamma                80.35(3)
_cell_formula_units_Z            2
_cell_length_a                   12.793(3)
_cell_length_b                   14.864(3)
_cell_length_c                   15.340(3)
_cell_measurement_temperature    180(2)
_cell_volume                     2554.0(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0777
_diffrn_reflns_av_sigmaI/netI    0.1077
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20787
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    2.142
_exptl_absorpt_correction_T_max  0.8306
_exptl_absorpt_correction_T_min  0.3155
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1286
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.468
_refine_diff_density_min         -1.718
_refine_diff_density_rms         0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         8998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1316
_reflns_number_gt                6142
_reflns_number_total             8998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001322f.txt
_cod_data_source_block           dw0002
_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 
;
_cod_original_cell_volume        2554.0(9)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C47.50 H66 N8 O4 Sb4'
_cod_database_code               7009474