Heavier N-heterocyclic half-sandwich tetrylenes
Bischoff, Inga-Alexandra; Morgenstern, Bernd; Schäfer, André; Chemical Communications  (2022) –; doi:10.1039/D2CC03107H

data_7130352
_publ_section_title
;
 Heavier N-heterocyclic half-sandwich tetrylenes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03107H
_journal_year                    2022
_chemical_formula_moiety         'C26 H47 Ge N3 Si'
_chemical_formula_sum            'C26 H47 Ge N3 Si'
_chemical_formula_weight         502.34
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-07-04 deposited with the CCDC.	2022-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.6320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5226(3)
_cell_length_b                   16.5510(5)
_cell_length_c                   16.5994(7)
_cell_measurement_reflns_used    9305
_cell_measurement_temperature    132(2)
_cell_measurement_theta_max      31.53
_cell_measurement_theta_min      2.42
_cell_volume                     2797.19(17)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics    'DIAMOND, (Brandenburg, 2018)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement
;
SHELXL-2018/3 (Sheldrick, 2018),                                              
SHELXLe Rev 1000 (Huebschle et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      132(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 Apex, Nonius Kappa CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            57712
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.583
_diffrn_reflns_theta_min         1.767
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.155
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.7061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/n-Hexane'
_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.276
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         9376
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+1.4783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0816
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7758
_reflns_number_total             9376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03107h3.cif
_cod_data_source_block           4586_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7130352
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.689
_shelx_estimated_absorpt_t_max   0.741
_shelx_res_checksum              41148
_shelx_hkl_checksum              69443