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_4323646
_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            'C28 H46 N4 Sn3'
_chemical_formula_weight         794.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.67(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.582(5)
_cell_length_b                   13.997(4)
_cell_length_c                   21.647(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_volume                     3200(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  0.1163
_diffrn_reflns_av_sigmaI/netI    0.0962
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7489
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        -2%
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.345
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.959
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.030
_refine_ls_goodness_of_fit_obs   1.025
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5599
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.294
_refine_ls_restrained_S_obs      1.025
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_obs          0.0418
_refine_ls_shift/esd_max         -0.167
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+10.4406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1457
_refine_ls_wR_factor_obs         0.0939
_reflns_number_observed          3813
_reflns_number_total             5642
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970336i_1.cif
_cod_data_source_block           dw9608
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+10.4406P] 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^)+(0.0366P)^2^+10.4406P] 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        3199.7(20)
_cod_database_code               4323646