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_4078599
_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_sum            'C54 H46 Ge4'
_chemical_formula_weight         985.27
_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                 105.1780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1929(13)
_cell_length_b                   17.5573(18)
_cell_length_c                   19.868(2)
_cell_measurement_reflns_used    8965
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.32
_cell_volume                     4441.5(8)
_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      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36823
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    2.717
_exptl_absorpt_correction_T_max  0.6795
_exptl_absorpt_correction_T_min  0.5654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         8125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0841
_reflns_number_gt                6250
_reflns_number_total             8125
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300385n_si_001.cif
_cod_data_source_block           wein111
_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_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        4441.6(8)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4078599