A crystalline molecular gyrotop with germanium junctions between a phenylene rotor and alkyl spokes
Inagaki, Yusuke; Yamaguchi, Kentaro; Setaka, Wataru; RSC Adv.  (2014) –; doi:10.1039/C4RA11705K

data_7218644
_publ_section_title
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 A crystalline molecular gyrotop with germanium junctions between a
 phenylene rotor and alkyl spokes
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA11705K
_journal_year                    2014
_chemical_compound_source        no
_chemical_formula_moiety         'C48 H88 Ge2'
_chemical_formula_sum            'C48 H88 Ge2'
_chemical_formula_weight         810.36
_chemical_melting_point          517.6(5)
_chemical_name_common            GeMolecularGyrotop
_chemical_name_systematic        GeMolecularGyrotop
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 118.979(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.056(10)
_cell_length_b                   11.558(4)
_cell_length_c                   19.190(7)
_cell_measurement_reflns_used    1428
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      16.30
_cell_measurement_theta_min      2.43
_cell_volume                     5056(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      300(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0902
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10770
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    1.216
_exptl_absorpt_correction_T_max  0.7930
_exptl_absorpt_correction_T_min  0.6420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS  Bruker'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1760
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/tetrahydrofuran'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.35(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6828
_refine_ls_number_restraints     294
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.1889
_refine_ls_R_factor_gt           0.0712
_refine_ls_shift/su_max          0.163
_refine_ls_shift/su_mean         0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1254P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1778
_refine_ls_wR_factor_ref         0.2648
_reflns_number_gt                1984
_reflns_number_total             6828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra11705k2.cif
_cod_data_source_block           GeC14Phcage
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '244-245 deg. C' was changed to
'517.6(5)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Monoclinic' changed to
'monoclinic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 
;
_cod_original_sg_symbol_H-M      'C c  '
_cod_database_code               7218644