Crystalline (NN)C‒M(NN) complexes: synthesis, structure, bonding and lability [M = Si, Ge, Sn or Pb; (NN) = 1,2-(ButCH2N)2C6H4]
Gehrhus, Barbara; Hitchcock, Peter B.; Lappert, Michael F.; Journal of the Chemical Society, Dalton Transactions  (2000) 3094–; doi:10.1039/b005216g

data_7010035
_publ_section_title
;
 Crystalline (NN)C--M(NN) complexes: synthesis, structure, bonding and
 lability [M&#x2005;=&#x2005;Si, Ge, Sn or Pb;
 (NN)&#x2005;=&#x2005;1,2-(ButCH2N)2C6H4]
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3094
_journal_paper_doi               10.1039/b005216g
_journal_year                    2000
_chemical_formula_sum            'C33 H52 N4 Sn'
_chemical_formula_weight         623.48
_chemical_name_common            '[C6H4(NCH2tBu)2CSn(NCH2tBu)2C6H4]'
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.39(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.396(3)
_cell_length_b                   16.059(5)
_cell_length_c                   20.20(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     3281(7)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'ORTEP3-for Windows'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_method       \w--2\q
_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  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0897
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6096
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.00078(16)
_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   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1079
_reflns_number_gt                4063
_reflns_number_total             5767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005216g.txt
_cod_data_source_block           GERHUS-HITCHCOCK-LAPPERT-10
_cod_original_cell_volume        3281(6)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010035