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_7009475
_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            'C28 H56 N6 Na Sb3'
_chemical_formula_weight         865.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.82(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.599(2)
_cell_length_b                   21.379(4)
_cell_length_c                   17.097(3)
_cell_measurement_temperature    180(2)
_cell_volume                     3457.2(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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0881
_diffrn_reflns_av_sigmaI/netI    0.0953
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6596
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         4.00
_exptl_absorpt_coefficient_mu    2.366
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.644
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.831
_refine_diff_density_min         -1.814
_refine_diff_density_rms         0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4499
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0787
_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^)+(0.1522P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1986
_refine_ls_wR_factor_ref         0.2259
_reflns_number_gt                3116
_reflns_number_total             4499
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001322f.txt
_cod_data_source_block           dw9825
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        3457.2(11)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7009475