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_4301669
_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         'C70 H89 Ge2 N, C6 H14'
_chemical_formula_sum            'C76 H103 Ge2 N'
_chemical_formula_weight         1175.82
_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                 112.2680(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.5935(18)
_cell_length_b                   12.9828(10)
_cell_length_c                   22.8808(18)
_cell_measurement_reflns_used    7896
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.35
_cell_volume                     6485.9(9)
_computing_cell_refinement       'SAINT (7.46A) (Bruker, 2006)'
_computing_data_collection       'SMART (Version 5.054) (Bruker, 2002)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART1000 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  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            80681
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         0.93
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/2 (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       multifact
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         14980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0491P)^2^+6.7076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1058
_reflns_number_gt                11937
_reflns_number_total             14980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801713v_si_001_3.cif
_cod_data_source_block           p21c
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4301669