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#$Date: 2024-02-04 13:09:22 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289343 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/24/7132449.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7132449
loop_
_publ_author_name
'Eisner, Teresa'
'Kostenko, Arseni'
'J Kiefer, Fiona'
'Inoue, Shigeyoshi'
_publ_section_title
;
 Synthesis and isolation of a cyclic bis-vinyl germylene via a
 diazoolefin adduct of germylene dichloride.
;
_journal_issue                   5
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              558
_journal_page_last               561
_journal_paper_doi               10.1039/d3cc05090d
_journal_volume                  60
_journal_year                    2024
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C28 H36 Cl2 Ge N4'
_chemical_formula_sum            'C28 H36 Cl2 Ge N4'
_chemical_formula_weight         572.10
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     dual
_audit_update_record
;
2023-10-16 deposited with the CCDC.	2023-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.330(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1689(6)
_cell_length_b                   16.1850(9)
_cell_length_c                   22.5667(13)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    100
_cell_measurement_theta_max      37.85
_cell_measurement_theta_min      2.56
_cell_volume                     3339.3(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1084
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            700304
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         46.58
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    1.097
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2, Bruker, 2016'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.862
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         29697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[Σ²(FO²)+(0.0561P)²+0.6647P] WHERE P=(FO²+2FC²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1203
_reflns_number_gt                21195
_reflns_number_total             29697
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            d3cc05090d2.cif
_cod_data_source_block           jk_ter1_0ma
_cod_depositor_comments
'Adding full bibliography for 7132449--7132451.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7132449
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C26(H26), C23(H23), C11(H11), C14(H14)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C19(H19), C9(H9), C21(H21), C8(H8), C20(H20), C7(H7)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C24(H24A,H24B,H24C), C28(H28A,H28B,
 H28C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C12(H12A,H12B,H12C), C16(H16A,
 H16B,H16C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 158 electrons were 
found in a volume of 740Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1[C4H8O] (THF) per Asymmetric Unit 
which account for 160 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
