Synthetic, Structural, and Physical Investigations of the Large Linear and Branched Oligogermanes Ph3GeGePh2GePh2GePh2H, Ge5Ph12, and (Ph3Ge)4Ge
Samanamu, Christian R.; Amadoruge, Monika L.; Schrick, Aaron C.; Chen, Chao; Golen, James A.; Rheingold, Arnold L.; Materer, Nicholas F.; Weinert, Charles S.; Organometallics 31 (2012) 4374–; doi:10.1021/om300385n

data_4078602
_publ_section_title
;
 Synthetic, Structural, and Physical Investigations of the Large Linear
 and Branched Oligogermanes Ph3GeGePh2GePh2GePh2H, Ge5Ph12, and (Ph3Ge)4Ge
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              4374
_journal_paper_doi               10.1021/om300385n
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C20 H17 Ge N'
_chemical_formula_sum            'C20 H17 Ge N'
_chemical_formula_weight         343.96
_chemical_melting_point          ?
_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                92.021(3)
_cell_angle_beta                 108.696(3)
_cell_angle_gamma                98.341(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4123(19)
_cell_length_b                   9.4402(19)
_cell_length_c                   9.779(2)
_cell_measurement_reflns_used    1962
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.93
_cell_measurement_theta_min      2.19
_cell_volume                     811.2(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Bruker Apex'
_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  0.0862
_diffrn_reflns_av_sigmaI/netI    0.1099
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9828
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    1.884
_exptl_absorpt_correction_T_max  0.8340
_exptl_absorpt_correction_T_min  0.7280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       'not measured'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0410P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                2699
_reflns_number_total             3695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300385n_si_004.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_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 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4078602