Silicon(IV) tetraazachlorin - an unusual cycloaddition product from 3,4-diphenyl-1<i>H</i>-pyrrole-2,5-diimine.
Rychikhina, Ekaterina D.; Ivanova, Svetlana S.; Somov, Nikolay V.; Lazovskiy, Dmitry A.; Stuzhin, Pavel A.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11822–11827; doi:10.1039/d5dt01113b

data_1575115
_publ_section_title
;
 Silicon(IV) tetraazachlorin - an unusual cycloaddition product from
 3,4-diphenyl-1<i>H</i>-pyrrole-2,5-diimine.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11822
_journal_page_last               11827
_journal_paper_doi               10.1039/d5dt01113b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_sum            'C104 H99 N10 O3 Si3'
_chemical_formula_weight         1621.20
_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
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2023-6-14
_audit_creation_method           CifMake
_audit_update_record
;
2025-05-06 deposited with the CCDC.	2025-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.594(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3522(4)
_cell_length_b                   35.9188(6)
_cell_length_c                   16.5121(4)
_cell_measurement_reflns_used    50916
_cell_measurement_temperature    106(10)
_cell_measurement_theta_max      27.3110
_cell_measurement_theta_min      2.2910
_cell_volume                     8672.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    Mercury
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      106(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            155338
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.190
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.143
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       block
_exptl_crystal_F_000             3436
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.250
_refine_diff_density_max         1.783
_refine_diff_density_min         -1.829
_refine_diff_density_rms         0.094
_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     1061
_refine_ls_number_reflns         17717
_refine_ls_number_restraints     182
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_gt           0.1007
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.1415P)^2^+26.5286P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2680
_refine_ls_wR_factor_ref         0.2891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13541
_reflns_number_total             17717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01113b2.cif
_cod_data_source_block           SiPzPh2
_cod_depositor_comments          'Adding full bibliography for 1575115.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1575115