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_7010034
_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 Ge N4'
_chemical_formula_weight         577.38
_chemical_name_common            '[C6H4((NCH2tBu)2GeC(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
_cell_angle_alpha                90.00
_cell_angle_beta                 101.85(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.146(2)
_cell_length_b                   16.243(9)
_cell_length_c                   20.054(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     3234(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       'omega-2theta scan'
_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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0604
_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            6018
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0010(2)
_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_all   1.055
_refine_ls_goodness_of_fit_obs   1.081
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         5681
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_restrained_S_obs      1.081
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_obs          0.0424
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+2.0968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1036
_refine_ls_wR_factor_obs         0.0918
_reflns_number_observed          4370
_reflns_number_total             5683
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b005216g.txt
_cod_data_source_block           GERHUS-HITCHCOCK-LAPPERT-9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+2.0968P] 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^)+(0.0349P)^2^+2.0968P] 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        3234.5(20)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010034