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_4301667
_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         'C60 H78 Ge2 N2, 4(C7 H8)'
_chemical_formula_sum            'C88 H110 Ge2 N2'
_chemical_formula_weight         1340.96
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.599(1)
_cell_angle_beta                 102.819(1)
_cell_angle_gamma                103.691(1)
_cell_formula_units_Z            1
_cell_length_a                   12.0284(9)
_cell_length_b                   13.1937(10)
_cell_length_c                   13.6696(10)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.87
_cell_volume                     1875.0(2)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16085
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.8870
_exptl_absorpt_correction_T_min  0.6739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2 (Sheldrick, 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_meas      0
_exptl_crystal_description       multi-faceted
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.206
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         8567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0586P)^2^+0.6844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                7652
_reflns_number_total             8567
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801713v_si_001_1.cif
_cod_data_source_block           xp6fmi
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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               4301667