Synthesis and structural characterization of a novel asymmetric distannene [{1-[N(But)C(SiMe3)C(H)]-2-[N(But)(SiMe3)CC(H)]C6H4}Sn\ρightarrow Sn{1,2-[N(But)(SiMe3)CC(H)]2C6H4}]
Leung, Wing-Por; Cheng, Hui; Huang, Rong-Bin; Yang, Qing-Chuan; Mak, Thomas C. W.; Chemical Communications  (2000) 451–; doi:10.1039/b000268m

data_7110842
_publ_section_title
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 Synthesis and structural characterization of a novel asymmetric
 distannene
 [{1-[N(But)C(SiMe3)C(H)]-2-[N(But)(SiMe3)CC(H)]C6H4}Sn\\rightarrow
 Sn{1,2-[N(But)(SiMe3)CC(H)]2C6H4}]
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_journal_issue                   6
_journal_name_full               'Chemical Communications'
_journal_page_first              451
_journal_paper_doi               10.1039/b000268m
_journal_year                    2000
_chemical_formula_sum            'C52 H92 N4 O Si4 Sn2'
_chemical_formula_weight         1139.04
_chemical_melting_point          392.0(10)
_chemical_name_systematic
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 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.004(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.108(1)
_cell_length_b                   36.869(3)
_cell_length_c                   14.320(1)
_cell_measurement_temperature    294(2)
_cell_volume                     6174.7(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omege 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  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42889
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.922
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8559
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.00033(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         15255
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.979
_refine_ls_shift/su_mean         0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1435
_reflns_number_gt                9055
_reflns_number_total             15255
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b000268msup1.cif
_cod_data_source_block           a
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '391-393' was changed to '392.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        6174.7(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7110842