Spirocyclic germanes via transannular insertion reactions of vinyl germylenes into Si-Si bonds.
Walewska, Małgorzata; Baumgartner, Judith; Marschner, Christoph; Albers, Lena; Müller, Thomas; Dalton transactions (Cambridge, England : 2003) 47 (2018) 5985–5996; doi:10.1039/c8dt00315g

data_7045917
_publ_section_title
;
 Spirocyclic germanes via transannular insertion reactions of vinyl
 germylenes into Si-Si bonds.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5985
_journal_page_last               5996
_journal_paper_doi               10.1039/c8dt00315g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C30 H58 Ge3 Si6'
_chemical_formula_weight         805.07
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-01-27 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.083(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.817(3)
_cell_length_b                   35.902(9)
_cell_length_c                   10.823(3)
_cell_measurement_reflns_used    5995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      5.375
_cell_measurement_theta_min      4.400
_cell_volume                     4179.5(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SMART APEX'
_diffrn_measurement_method       '\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  0.0948
_diffrn_reflns_av_sigmaI/netI    0.0859
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            33243
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    2.333
_exptl_absorpt_correction_T_max  0.9124
_exptl_absorpt_correction_T_min  0.6278
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
;
_refine_diff_density_max         2.036
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         8542
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0894
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+15.8027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1831
_refine_ls_wR_factor_ref         0.1923
_reflns_number_gt                6742
_reflns_number_total             8542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt00315g4.cif
_cod_data_source_block           1103j
_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/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 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7045912--7045917.cif.
;
_cod_original_cell_volume        4179.6(19)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7045917