Divalent Germanium Compound with a Radical-Anionic Ligand: Molecular Structures of (dpp-BIAN).-GeCl and Its Hydrochloration Products [(dpp-BIAN)(H)2].+[GeCl3]- and [{(dpp-BIAN)(H)2.+}2(Cl-)]+[GeCl3]- (dpp-BIAN = 1,2-Bis{(2,6-diisopropylphenyl)imino}acenaphthene)
Igor L. Fedushkin; Natalie M. Khvoinova; Andrey Yu. Baurin; Georgii K. Fukin; Vladimir K. Cherkasov; Mikhail P. Bubnov; Inorganic Chemistry 43 (2004) 7807–7815; doi:10.1021/ic048801g

data_4312055
_publ_section_title
;
 Divalent Germanium Compound with a Radical-Anionic Ligand: Molecular
 Structures of (dpp-BIAN).-GeCl and Its Hydrochloration Products
 [(dpp-BIAN)(H)2].+[GeCl3]- and [{(dpp-BIAN)(H)2.+}2(Cl-)]+[GeCl3]-
 (dpp-BIAN = 1,2-Bis{(2,6-diisopropylphenyl)imino}acenaphthene)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7807
_journal_page_last               7815
_journal_paper_doi               10.1021/ic048801g
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C36 H42 Cl3 Ge N2'
_chemical_formula_weight         681.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_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            4
_cell_length_a                   11.131(3)
_cell_length_b                   13.696(2)
_cell_length_c                   22.431(5)
_cell_measurement_reflns_used    800
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2
_cell_volume                     3419.6(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16088
_diffrn_reflns_theta_full        23.31
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.157
_exptl_absorpt_correction_T_max  0.9552
_exptl_absorpt_correction_T_min  0.8276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1998a)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.008(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         4934
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0722
_reflns_number_gt                4344
_reflns_number_total             4934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048801gsi20040830_045626_2.cif
_cod_data_source_block           compound_2
_cod_depositor_comments
;
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               4312055