Preparation of a high-coordinated-silicon-centered spiro-cyclic compound.
Kushvaha, Saroj Kumar; Gorantla, Sai Manoj N. V. T.; Kallenbach, Paula; Herbst-Irmer, Regine; Stalke, Dietmar; Roesky, Herbert W.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11410–11416; doi:10.1039/d4dt00627e

data_7716338
_publ_section_title
;
 Preparation of a high-coordinated-silicon-centered spiro-cyclic compound.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11410
_journal_page_last               11416
_journal_paper_doi               10.1039/d4dt00627e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C27 H33 Cl N2 Si2'
_chemical_formula_sum            'C27 H33 Cl N2 Si2'
_chemical_formula_weight         477.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-09-04 deposited with the CCDC.	2024-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.543(4)
_cell_length_b                   9.225(2)
_cell_length_c                   22.485(3)
_cell_measurement_reflns_used    9028
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.1995
_cell_measurement_theta_min      2.347
_cell_volume                     5298.2(16)
_computing_cell_refinement       'Bruker SAINT V8.40B'
_computing_data_collection       'Bruker APEX2 v2012.2'
_computing_data_reduction        'Bruker SAINT V8.40B'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT(Sheldrick,Acta Cryst.(2015)A71,3-8)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_type            'Bruker Photon III C7 CMOS'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            200799
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.393
_diffrn_reflns_theta_min         1.594
_diffrn_source                   'Incoatec Microsource'
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Flack x determined using 5892 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.104(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         13285
_refine_ls_number_restraints     4077
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0336P)^2^+1.2311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.949
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                12607
_reflns_number_total             13285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00627e2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7716338--7716339.cif.'
_cod_database_code               7716338
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.919
_shelx_estimated_absorpt_t_max   0.968
_shelx_res_checksum              20041
_shelx_hkl_checksum              62903