Azido Derivatives of Germanium(II) and Tin(II): Syntheses and Characterization of [(Mes)2DAP]GeN3, [(Mes)2DAP]SnN3, and the Corresponding Chloro Analogues Featuring Heterocyclic Six-π-Electron Ring Systems (where [(Mes)2DAP] = {N(Mes)C(Me)}2CH)
Ashley E. Ayers; Thomas M. Klapötke; H. V. Rasika Dias; Inorganic Chemistry 40 (2001) 1000–1005; doi:10.1021/ic001078j

data_4319326
_publ_section_title
;
 Azido Derivatives of Germanium(II) and Tin(II): Syntheses and
 Characterization of [(Mes)2DAP]GeN3, [(Mes)2DAP]SnN3, and the
 Corresponding Chloro Analogues Featuring Heterocyclic Six-\p-Electron
 Ring Systems (where [(Mes)2DAP] = {N(Mes)C(Me)}2CH)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1000
_journal_page_last               1005
_journal_paper_doi               10.1021/ic001078j
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C23 H29 Cl Ge N2'
_chemical_formula_weight         441.52
_chemical_name_common            '[(Mes)2DAP]GeCl'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 114.144(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.967(4)
_cell_length_b                   12.369(4)
_cell_length_c                   14.5548(13)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      12.47
_cell_measurement_theta_min      5.27
_cell_volume                     4430.1(16)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_method       '\w 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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3376
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.84
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.513
_exptl_absorpt_correction_T_max  0.9216
_exptl_absorpt_correction_T_min  0.7519
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelpipeds
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.43
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         2810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+5.9208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                2582
_reflns_number_total             2810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001078j_1.cif
_cod_data_source_block           rd254
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4430.2(17)
_cod_database_code               4319326