Cooperative and non-cooperative additions involving a silicon atom and a redox-active ligand.
Dodonov, Vladimir A.; Kryuchenkova, Alina A.; Kushnerova, Olga A.; Baranov, Evgeny V.; Zhao, Yanxia; Osmanov, Vladimir K.; Fedushkin, Igor L.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3921–3929; doi:10.1039/d4dt03409k

data_7717860
_publ_section_title
;
 Cooperative and non-cooperative additions involving a silicon atom and a
 redox-active ligand.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3921
_journal_page_last               3929
_journal_paper_doi               10.1039/d4dt03409k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_sum            'C50 H50 N2 Si'
_chemical_formula_weight         707.01
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-10-31 deposited with the CCDC.	2025-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.055(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5811(3)
_cell_length_b                   16.4451(4)
_cell_length_c                   16.0981(3)
_cell_measurement_reflns_used    10104
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4530
_cell_measurement_theta_min      1.8730
_cell_volume                     4073.46(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.76a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.76a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.76a (Rigaku OD, 2022)'
_computing_structure_refinement  SHELXL-2018/3
_computing_structure_solution    SHELXT-2014/5
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0704
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 1.000
_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       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30457
_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         27.484
_diffrn_reflns_theta_min         1.812
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.76a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_description       prism
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.480
_exptl_crystal_size_min          0.410
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         9350
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0566P)^2^+1.7257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1364
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6841
_reflns_number_total             9350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03409k3.cif
_cod_data_source_block           sibianphccph
_cod_depositor_comments
'Adding full bibliography for 7717857--7717862.cif.'
_cod_original_cell_volume        4073.45(15)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7717860
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.950
_shelx_estimated_absorpt_t_max   0.963
_oxdiff_exptl_absorpt_empirical_full_min 0.920
_oxdiff_exptl_absorpt_empirical_full_max 1.181
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              63103