N-H and N=C Bond Formation via Germanium(III) Diradicaloid Intermediates and C-S Bond Cleavage in Reactions of the Digermyne Ar'GeGeAr' (Ar' = C6H3-2,6-(C6H3-2,6-Pri2)2) with Azides
Xinping Wang; Chengbao Ni; Zhongliang Zhu; James C. Fettinger; Philip P. Power; Inorganic Chemistry 48 (2009) 2464–2470; doi:10.1021/ic801713v

data_4301668
_publ_section_title
;
N-H and N=C Bond Formation via Germanium(III) Diradicaloid Intermediates
and C-S Bond Cleavage in Reactions of the Digermyne Ar'GeGeAr' (Ar'
= C6H3-2,6-(C6H3-2,6-Pri2)2) with Azides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2464
_journal_page_last               2470
_journal_paper_doi               10.1021/ic801713v
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C84 H130 Ge2 N2 Sn2'
_chemical_formula_sum            'C84 H130 Ge2 N2 Sn2'
_chemical_formula_weight         1550.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.0657(11)
_cell_length_b                   21.0954(10)
_cell_length_c                   32.2509(15)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      2.62
_cell_volume                     15692.6(13)
_computing_cell_refinement       'SAINT (7.46A) (Bruker, 2006)'
_computing_data_collection       'Apex2 (2.2-0) (Bruker, 2007)'
_computing_data_reduction        'SAINT (7.46A) (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0929
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            130952
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    1.431
_exptl_absorpt_correction_T_max  0.8678
_exptl_absorpt_correction_T_min  0.8425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2 (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Multi-faceted
_exptl_crystal_F_000             6496
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.997
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         17978
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0331P)^2^+3.4198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                12774
_reflns_number_total             17978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801713v_si_001_2.cif
_cod_data_source_block           xp7ffmi
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4301668