Syntheses and Structures of [Sn{NR}2{Sn(μ-NMe2)}2]: Model Intermediates in the Formation of Imido Group 14 Cages and Rings [R = 2,6-Pri2C6H3(Dipp), 2,4,6-Me3C6H2(Mes)]
Robert E. Allan; Michael A. Beswick; Georgina R. Coggan; Paul R. Raithby; Andrew E. H. Wheatley; Dominic S. Wright; Inorganic Chemistry 36 (1997) 5202–5205; doi:10.1021/ic970336i

data_4323647
_publ_section_title
;
 Syntheses and Structures of [Sn{NR}2{Sn(\m-NMe2)}2]: Model Intermediates
 in the Formation of Imido Group 14 Cages and Rings [R =
 2,6-Pri2C6H3(Dipp), 2,4,6-Me3C6H2(Mes)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5202
_journal_page_last               5205
_journal_paper_doi               10.1021/ic970336i
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C73 H110 N12 Sn9'
_chemical_formula_weight         2223.94
_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
_cell_angle_alpha                103.72(3)
_cell_angle_beta                 100.36(2)
_cell_angle_gamma                69.51(2)
_cell_formula_units_Z            2
_cell_length_a                   15.442(4)
_cell_length_b                   19.919(6)
_cell_length_c                   15.201(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_volume                     4231(2)
_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  0.0520
_diffrn_reflns_av_sigmaI/netI    0.1245
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13825
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        -0.9%
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.654
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_F_000             2164
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.663
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.023
_refine_ls_goodness_of_fit_obs   1.073
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         13233
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.280
_refine_ls_restrained_S_obs      1.073
_refine_ls_R_factor_all          0.1255
_refine_ls_R_factor_obs          0.0584
_refine_ls_shift/esd_max         -1.005
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+28.0932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1549
_refine_ls_wR_factor_obs         0.1027
_reflns_number_observed          8361
_reflns_number_total             13268
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970336i_2.cif
_cod_data_source_block           dw9702
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+28.0932P] 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^)+(0.0209P)^2^+28.0932P] 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        4230.7(22)
_cod_database_code               4323647