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_7028175
_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            'C44 H82 N6 O2 Rb Sb3'
_chemical_formula_weight         1177.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 103.52(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.733(4)
_cell_length_b                   11.2981(12)
_cell_length_c                   21.075(4)
_cell_measurement_reflns_used    41
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      12.48
_cell_measurement_theta_min      5.29
_cell_volume                     5262.9(15)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\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  0.0666
_diffrn_reflns_av_sigmaI/netI    0.0859
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5570
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        17.87
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.485
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.20mm
_exptl_crystal_size_mid          0.32mm
_exptl_crystal_size_min          0.40mm
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.028
_refine_ls_goodness_of_fit_obs   1.083
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4628
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.039
_refine_ls_restrained_S_obs      1.095
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_obs          0.0506
_refine_ls_shift/esd_max         -0.763
_refine_ls_shift/esd_mean        0.063
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+5.5990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1214
_refine_ls_wR_factor_obs         0.0972
_reflns_number_observed          2779
_reflns_number_total             4630
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            j708496sup1.cif
_cod_data_source_block           RbSb
_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^)+(0.0488P)^2^+5.5990P] 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^)+(0.0488P)^2^+5.5990P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7028175