Synthesis and structure of [{Sn4(NBut)3P}{Sn4(NBut)3(OSiMe3)}]; a low-oxidation state p-block metal complex containing a P3− anion
Mosquera, Marta E. G.; Hopkins, Alexander D.; Raithby, Paul R.; Rothenberger, Alexander; Woods, Anthony D.; Wright, Dominic S.; Steiner, Alexander; Chemical Communications  (2001) 327–; doi:10.1039/b008108f

data_7111164
_publ_section_title
;
 Synthesis and structure of [{Sn4(NBut)3P}{Sn4(NBut)3(OSiMe3)}]; a
 low-oxidation state p-block metal complex containing a P3&#x2212; anion
;
_journal_issue                   4
_journal_name_full               'Chemical Communications'
_journal_page_first              327
_journal_paper_doi               10.1039/b008108f
_journal_year                    2001
_chemical_formula_sum            'C27 H63 N6 O P Si Sn8'
_chemical_formula_weight         1496.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           8
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 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                 116.00(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.453(3)
_cell_length_b                   15.280(3)
_cell_length_c                   12.736(3)
_cell_measurement_reflns_used    15443
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2353.1(11)
_computing_molecular_graphics    'SHELXTL-PLUS (sheldrick, 1991)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    TeXsan
_diffrn_ambient_temperature      220(2)
_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  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10543
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    4.258
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   SORTAV
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.112
_exptl_crystal_description       Block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.799
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.53(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.056
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_hydrogen_treatment    'Riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         5238
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      2.227
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_obs          0.0425
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+20.0967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1928
_refine_ls_wR_factor_obs         0.0875
_reflns_number_observed          4605
_reflns_number_total             5252
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b008108fsup1.cif
_cod_data_source_block           dw9924
_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^)+(0.0245P)^2^+20.0967P] 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^)+(0.0245P)^2^+20.0967P] 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        2353.1(8)
_cod_original_sg_symbol_H-M      Cm
_cod_database_code               7111164