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_4319329
_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 N5 Sn'
_chemical_formula_weight         494.20
_chemical_name_common            '[(Mes)2DAP]SnN3'
_chemical_name_systematic
; 
 ? 
;
_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                 108.285(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8207(11)
_cell_length_b                   15.254(2)
_cell_length_c                   14.9234(16)
_cell_measurement_reflns_used    41
_cell_measurement_temperature    228(2)
_cell_measurement_theta_max      12.48
_cell_measurement_theta_min      4.91
_cell_volume                     2338.9(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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      228(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3037
_diffrn_reflns_theta_full        21.99
_diffrn_reflns_theta_max         21.99
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        5.98
_diffrn_standards_interval_count 145
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.110
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.50
_refine_diff_density_max         3.222
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.0014(4)
_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   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         2863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0466P)^2^+12.9987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                2702
_reflns_number_total             2863
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001078j_4.cif
_cod_data_source_block           uta-sn
_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        2338.8(5)
_cod_database_code               4319329