Germanium- and Tin-Bridged Diazulenylmethyl Cations: Effects of the Group 14 Element on the Structure and Properties of the π-Extended Cation
Murai, Masahito; Ito, Mako; Takahashi, Satoshi; Yamaguchi, Shigehiro; Dalton Transactions  (2023) –; doi:10.1039/D3DT01491F

data_7713115
_publ_section_title
;
 Germanium- and Tin-Bridged Diazulenylmethyl Cations: Effects of the Group
 14 Element on the Structure and Properties of the \p-Extended Cation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01491F
_journal_year                    2023
_chemical_formula_sum            'C23 H19 F6 Ge P'
_chemical_formula_weight         512.94
_chemical_name_common            'Ge-bridged diazulenylmethyl cation'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-03-28 deposited with the CCDC.	2023-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.072(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.1631(6)
_cell_length_b                   11.2974(2)
_cell_length_c                   13.8266(3)
_cell_measurement_reflns_used    15074
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.7820
_cell_measurement_theta_min      1.5840
_cell_volume                     4159.24(16)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4129
_diffrn_reflns_av_R_equivalents  0.0999
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            46342
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        14.344
_diffrn_reflns_theta_max         15.552
_diffrn_reflns_theta_min         1.585
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/hexane'
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 3966 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.284(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         9517
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0442
_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/[\s^2^(Fo^2^)+6.6843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.0972
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                9049
_reflns_number_total             9517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01491f2.cif
_cod_data_source_block           04_MI01__autored_a
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7713115
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.963
_shelx_res_checksum              94539
_shelx_hkl_checksum              60676