Complementary bonding analysis of the N – Si interaction in pentacoordinated silicon compounds using quantum crystallography
Fugel, Malte; Ponomarenko, Maksym; Hesse, Maxie F.; Malaspina, Lorraine Andrade; Kleemiss, Florian; Sugimoto, Kunihisa; Genoni, Alessandro; Röschenthaler, Gerd-Volker; Grabowsky, Simon; Dalton Transactions  (2019) –; doi:10.1039/C9DT02772F

data_7701298
_publ_section_title
;
 Complementary bonding analysis of the N -- Si interaction in
 pentacoordinated silicon compounds using quantum crystallography
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT02772F
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '2(C20 H23 F N Si), 2(B F4), C H2 Cl2'
_chemical_formula_sum            'C41 H48 B2 Cl2 F10 N2 Si2'
_chemical_formula_weight         907.51
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-06-13T14:24:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-07-02 deposited with the CCDC.    2019-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.58(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.131(3)
_cell_length_b                   7.7980(16)
_cell_length_c                   21.291(4)
_cell_measurement_reflns_used    154629
_cell_measurement_temperature    20(10)
_cell_measurement_theta_max      26.51
_cell_measurement_theta_min      0.55
_cell_measurement_wavelength     0.4015
_cell_volume                     2149.7(8)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction
'CrystalClear (Rigaku/MSC Inc., 2006), SORTAV (Blessing, 1995)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      20(10)
_diffrn_detector                 'SPring-8 BL02B1 Curved Imaging Plate'
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'quarter \C-circle diffractometer'
_diffrn_measurement_device_type  IPDSC-Q
_diffrn_measurement_method       'phi or omega oscillation scans'
_diffrn_orient_matrix_type       fs_process
_diffrn_orient_matrix_UB_11      0.001761
_diffrn_orient_matrix_UB_12      -0.003396
_diffrn_orient_matrix_UB_13      -0.046758
_diffrn_orient_matrix_UB_21      -0.014076
_diffrn_orient_matrix_UB_22      -0.126055
_diffrn_orient_matrix_UB_23      -0.000417
_diffrn_orient_matrix_UB_31      -0.075921
_diffrn_orient_matrix_UB_32      0.023292
_diffrn_orient_matrix_UB_33      -0.009073
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4015
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            134595
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        13.94
_diffrn_reflns_theta_max         26.495
_diffrn_reflns_theta_min         0.963
_diffrn_source                   'SPring-8 BL02'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.647
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     575
_refine_ls_number_reflns         44848
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1280P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.1818
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                34497
_reflns_number_total             44848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02772f2.cif
_cod_data_source_block           F_bridged_prot
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               7701298
_shelx_res_checksum              17396