Syntheses, Structures, and Electronic Properties of the Branched Oligogermanes (Ph3Ge)3GeH and (Ph3Ge)3GeX (X = Cl, Br, I)†
Samanamu, Christian R.; Amadoruge, Monika L.; Yoder, Claude H.; Golen, James A.; Moore, Curtis E.; Rheingold, Arnold L.; Materer, Nicholas F.; Weinert, Charles S.; Organometallics 30 (2011) 1046–; doi:10.1021/om101091c

data_4064031
_publ_section_title
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 Syntheses, Structures, and Electronic Properties of the Branched
 Oligogermanes (Ph3Ge)3GeH and (Ph3Ge)3GeX (X = Cl, Br, I)&#x2020;
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_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1046
_journal_paper_doi               10.1021/om101091c
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C54 H45 Ge4 I, 0.5(C6 H6)'
_chemical_formula_sum            'C57 H48 Ge4 I'
_chemical_formula_weight         1150.21
_chemical_name_common            'COMPOUND 5'
_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                86.077(2)
_cell_angle_beta                 69.500(2)
_cell_angle_gamma                86.651(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7545(13)
_cell_length_b                   13.2977(12)
_cell_length_c                   15.1657(15)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.58
_cell_volume                     2402.0(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.908
_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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20853
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         1.44
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.159
_exptl_absorpt_correction_T_max  0.6487
_exptl_absorpt_correction_T_min  0.5056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1142
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         8994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+1.3979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0768
_reflns_number_gt                7324
_reflns_number_total             8994
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101091c_si_002.cif
_cod_data_source_block           wein99
_cod_depositor_comments
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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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064031
_alert_a_response_comment
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Although the extent of data collection is only 92 % the
quality of data is excellent.
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