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
Ashley E. Ayers; Dennis S. Marynick; H. V. Rasika Dias; Inorganic Chemistry 39 (2000) 4147–4151; doi:10.1021/ic000545u

data_4321340
_publ_section_title
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 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-\p-Electron Ring Systems
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_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 N5 Sn'
_chemical_formula_weight         364.02
_chemical_name_common            '[(n-Pr)2ATI]SnN3'
_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                90.465(14)
_cell_angle_beta                 91.358(12)
_cell_angle_gamma                111.820(9)
_cell_formula_units_Z            4
_cell_length_a                   7.9221(10)
_cell_length_b                   10.1385(13)
_cell_length_c                   19.989(3)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      12.52
_cell_measurement_theta_min      4.76
_cell_volume                     1489.8(4)
_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 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker P4'
_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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4691
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.04
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.710
_exptl_absorpt_correction_T_max  0.9997
_exptl_absorpt_correction_T_min  0.6263
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.0022(3)
_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   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         3672
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0308P)^2^+1.8491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                3412
_reflns_number_total             3672
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000545u_2.cif
_cod_data_source_block           rd242
_cod_depositor_comments
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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 
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_cod_database_code               4321340