Co-ordination of heavier alkali metals by polyimido antimony(III) ligands; syntheses and structures of [{Sb2(NC6H11)4}2M4] (M = Li or Na), Li[{(Me2N)Sb(μ-NC6H11)2}2Sb] and M[{(C6H11NH)Sb(μ-NC6H11)2}2Sb]·2thf (M = K or Rb)
Bashall, Alan; Beswick, Michael A.; Harmer, Christopher N.; Hopkins, Alexander D.; McPartlin, Mary; Paver, Michael A.; Raithby, Paul R.; Wright, Dominic S.; Journal of the Chemical Society, Dalton Transactions  (1998) 1389–; doi:10.1039/a708496j

data_7028173
_publ_section_title
;
 Co-ordination of heavier alkali metals by polyimido antimony(III)
 ligands; syntheses and structures of [{Sb2(NC6H11)4}2M4]
 (M&#x2005;=&#x2005;Li or Na), Li[{(Me2N)Sb(\m-NC6H11)2}2Sb] and
 M[{(C6H11NH)Sb(\m-NC6H11)2}2Sb]&#x00B7;2thf (M&#x2005;=&#x2005;K or Rb)
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1389
_journal_paper_doi               10.1039/a708496j
_journal_year                    1998
_chemical_formula_sum            'C48 H88 N8 Na4 Sb4'
_chemical_formula_weight         1356.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 91.28(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.560(4)
_cell_length_b                   18.455(11)
_cell_length_c                   25.187(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_volume                     11413(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       AFC5R
_diffrn_measurement_method       'omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.3178
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10631
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        -0.7%
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.942
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_F_000             5440
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.129
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.003
_refine_ls_goodness_of_fit_obs   1.134
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         10589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_restrained_S_obs      1.134
_refine_ls_R_factor_all          0.2537
_refine_ls_R_factor_obs          0.0764
_refine_ls_shift/esd_max         0.068
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2516
_refine_ls_wR_factor_obs         0.1727
_reflns_number_observed          4618
_reflns_number_total             10631
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            j708496sup1.cif
_cod_data_source_block           dw9607
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        11413.3(74)
_cod_original_sg_symbol_H-M      P2(1)/a
_cod_database_code               7028173