Synthesis of Silicon and Germanium-Containing Heterosumanenes via Rhodium-Catalyzed Cyclodehydrogenation of Silicon/Germanium-Hydrogen and Carbon-Hydrogen Bonds.
Zhou, Dandan; Gao, Ya; Liu, Bingxin; Tan, Qitao; Xu, Bin; Organic letters 19 (2017) 4628–4631; doi:10.1021/acs.orglett.7b02254

data_1547040
_publ_section_title
;
 Synthesis of Silicon and Germanium-Containing Heterosumanenes via
 Rhodium-Catalyzed Cyclodehydrogenation of Silicon/Germanium-Hydrogen and
 Carbon-Hydrogen Bonds.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              4628
_journal_page_last               4631
_journal_paper_doi               10.1021/acs.orglett.7b02254
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         C24H24Ge3
_chemical_formula_sum            'C24 H24 Ge3'
_chemical_formula_weight         530.20
_chemical_name_common            Ge-Sumanene
_chemical_name_systematic        Ge-Sumanene
_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                 93.774(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.121(7)
_cell_length_b                   20.805(12)
_cell_length_c                   19.049(11)
_cell_measurement_reflns_used    3580
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.89
_cell_measurement_theta_min      2.17
_cell_volume                     4793(5)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0798
_diffrn_reflns_av_sigmaI/netI    0.1005
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24352
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    3.744
_exptl_absorpt_correction_T_max  0.8960
_exptl_absorpt_correction_T_min  0.4546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flake
_exptl_crystal_F_000             2112
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         8480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0522P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1355
_reflns_number_gt                4633
_reflns_number_total             8480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol7b02254_si_002.cif
_cod_data_source_block           161205a_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        4794(5)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1547040