#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:11:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179316 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/13/4321339.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4321339
loop_
_publ_author_name
'Ashley E. Ayers'
'Dennis S. Marynick'
'H. V. Rasika Dias'
_publ_section_title
;
 Azido Derivatives of Low-Valent Group 14 Elements: Synthesis,
 Characterization, and Electronic Structure of [(n-Pr)2ATI]GeN3 and
 [(n-Pr)2ATI]SnN3 Featuring Heterobicyclic 10-π-Electron Ring Systems
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4147
_journal_page_last               4151
_journal_paper_doi               10.1021/ic000545u
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C13 H19 Ge N5'
_chemical_formula_weight         317.92
_chemical_name_common            '[(n-Pr)2ATI]GeN3'
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.848(13)
_cell_angle_beta                 109.876(10)
_cell_angle_gamma                100.905(12)
_cell_formula_units_Z            2
_cell_length_a                   7.5389(10)
_cell_length_b                   9.5627(16)
_cell_length_c                   11.0499(17)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      18.76
_cell_measurement_theta_min      5.44
_cell_volume                     726.0(2)
_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      198(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω 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  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2278
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.99
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.104
_exptl_absorpt_correction_T_max  0.9782
_exptl_absorpt_correction_T_min  0.6456
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0414(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         1764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0211
_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/[σ²(Fo²)+(0.0191P)²+0.6010P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0530
_reflns_number_gt                1720
_reflns_number_total             1764
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000545u_1.cif
_cod_data_source_block           rd241
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        726.01(19)
_cod_database_code               4321339
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge Ge 0.73700(3) 0.97818(3) 0.90278(2) 0.02350(14) Uani 1 1 d . . .
N1 N 0.6144(3) 0.7736(2) 0.87072(18) 0.0217(5) Uani 1 1 d . . .
N2 N 0.5033(3) 1.0426(2) 0.7834(2) 0.0337(5) Uani 1 1 d . . .
N3 N 0.4108(3) 0.9628(3) 0.6827(2) 0.0338(6) Uani 1 1 d . . .
N4 N 0.3163(4) 0.8869(3) 0.5874(3) 0.0642(8) Uani 1 1 d . . .
N9 N 0.8205(3) 0.9097(2) 0.76382(19) 0.0220(5) Uani 1 1 d . . .
C2 C 0.6474(3) 0.6875(3) 0.7835(2) 0.0217(6) Uani 1 1 d . . .
C3 C 0.5769(3) 0.5369(3) 0.7599(2) 0.0251(6) Uani 1 1 d . . .
H3A H 0.4969 0.5033 0.8067 0.030 Uiso 1 1 calc R . .
C4 C 0.6030(4) 0.4292(3) 0.6811(3) 0.0313(7) Uani 1 1 d . . .
H4A H 0.5420 0.3341 0.6850 0.038 Uiso 1 1 calc R . .
C5 C 0.7040(4) 0.4376(3) 0.5972(3) 0.0325(6) Uani 1 1 d . . .
H5A H 0.7046 0.3494 0.5509 0.039 Uiso 1 1 calc R . .
C6 C 0.8041(4) 0.5633(3) 0.5749(3) 0.0320(6) Uani 1 1 d . . .
H6A H 0.8624 0.5497 0.5123 0.038 Uiso 1 1 calc R . .
C7 C 0.8335(4) 0.7051(3) 0.6282(2) 0.0268(6) Uani 1 1 d . . .
H7A H 0.9101 0.7724 0.5968 0.032 Uiso 1 1 calc R . .
C8 C 0.7699(3) 0.7678(3) 0.7211(2) 0.0207(6) Uani 1 1 d . . .
C10 C 0.4967(3) 0.7195(3) 0.9460(2) 0.0255(6) Uani 1 1 d . . .
H10A H 0.5293 0.7914 1.0247 0.031 Uiso 1 1 calc R . .
H10B H 0.5297 0.6295 0.9751 0.031 Uiso 1 1 calc R . .
C11 C 0.2797(3) 0.6895(3) 0.8688(2) 0.0270(6) Uani 1 1 d . . .
H11A H 0.2487 0.6269 0.7848 0.032 Uiso 1 1 calc R . .
H11B H 0.2430 0.7815 0.8495 0.032 Uiso 1 1 calc R . .
C12 C 0.1625(4) 0.6161(3) 0.9436(3) 0.0370(7) Uani 1 1 d . . .
H12A H 0.0238 0.6024 0.8932 0.056 Uiso 1 1 calc R . .
H12B H 0.1958 0.6766 1.0280 0.056 Uiso 1 1 calc R . .
H12C H 0.1925 0.5221 0.9579 0.056 Uiso 1 1 calc R . .
C13 C 0.9466(4) 1.0066(3) 0.7143(2) 0.0262(6) Uani 1 1 d . . .
H13A H 0.8876 0.9923 0.6180 0.031 Uiso 1 1 calc R . .
H13B H 1.0736 0.9804 0.7379 0.031 Uiso 1 1 calc R . .
C14 C 0.9787(4) 1.1638(3) 0.7673(3) 0.0294(6) Uani 1 1 d . . .
H14A H 1.0409 1.1798 0.8635 0.035 Uiso 1 1 calc R . .
H14B H 0.8523 1.1911 0.7446 0.035 Uiso 1 1 calc R . .
C15 C 1.1072(4) 1.2575(3) 0.7104(3) 0.0361(7) Uani 1 1 d . . .
H15A H 1.1251 1.3593 0.7441 0.054 Uiso 1 1 calc R . .
H15B H 1.0457 1.2409 0.6152 0.054 Uiso 1 1 calc R . .
H15C H 1.2336 1.2324 0.7355 0.054 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge N9 79.68(8) . . ?
N1 Ge N2 96.92(9) . . ?
N9 Ge N2 95.87(9) . . ?
C2 N1 C10 122.7(2) . . ?
C2 N1 Ge 117.93(15) . . ?
C10 N1 Ge 119.29(16) . . ?
N3 N2 Ge 115.30(18) . . ?
N4 N3 N2 177.5(3) . . ?
C8 N9 C13 120.4(2) . . ?
C8 N9 Ge 117.06(15) . . ?
C13 N9 Ge 122.40(15) . . ?
N1 C2 C3 122.4(2) . . ?
N1 C2 C8 112.3(2) . . ?
C3 C2 C8 125.3(2) . . ?
C4 C3 C2 131.6(2) . . ?
C3 C4 C5 130.2(2) . . ?
C6 C5 C4 125.6(3) . . ?
C7 C6 C5 130.9(3) . . ?
C6 C7 C8 131.3(2) . . ?
N9 C8 C7 122.1(2) . . ?
N9 C8 C2 112.9(2) . . ?
C7 C8 C2 125.1(2) . . ?
N1 C10 C11 112.97(19) . . ?
C10 C11 C12 111.5(2) . . ?
N9 C13 C14 113.0(2) . . ?
C13 C14 C15 110.1(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge N1 1.9449(19) . ?
Ge N9 1.956(2) . ?
Ge N2 2.047(2) . ?
N1 C2 1.332(3) . ?
N1 C10 1.466(3) . ?
N2 N3 1.197(3) . ?
N3 N4 1.144(4) . ?
N9 C8 1.336(3) . ?
N9 C13 1.472(3) . ?
C2 C3 1.407(3) . ?
C2 C8 1.474(3) . ?
C3 C4 1.378(4) . ?
C4 C5 1.384(4) . ?
C5 C6 1.381(4) . ?
C6 C7 1.378(4) . ?
C7 C8 1.407(4) . ?
C10 C11 1.522(3) . ?
C11 C12 1.522(3) . ?
C13 C14 1.510(4) . ?
C14 C15 1.522(3) . ?
