Synthesis of six-coordinate mono-, bis-, and tris(tetrazolato) complexes via [3 + 2] cycloadditions of nitriles to silicon-bound azido ligands.
Portius, Peter; Davis, Martin; Dalton transactions (Cambridge, England : 2003) 45 (2016) 17141–17152; doi:10.1039/c6dt02867e

data_7040892
_publ_section_title
;
 Synthesis of six-coordinate mono-, bis-, and tris(tetrazolato) complexes
 via [3 + 2] cycloadditions of nitriles to silicon-bound azido ligands.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17141
_journal_page_last               17152
_journal_paper_doi               10.1039/c6dt02867e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C24 H18 N16 Si'
_chemical_formula_weight         558.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-14 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.2180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7377(5)
_cell_length_b                   10.3383(2)
_cell_length_c                   10.6088(2)
_cell_measurement_reflns_used    5857
_cell_measurement_temperature    87(2)
_cell_measurement_theta_max      27.1949
_cell_measurement_theta_min      2.1689
_cell_volume                     2461.60(9)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      87(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15600
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.518
_diffrn_reflns_theta_min         2.169
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.9912
_exptl_absorpt_correction_T_min  0.9459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.060
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.6541
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         2839
_refine_ls_number_restraints     603
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+1.5081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2337
_reflns_number_total             2839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02867e2.cif
_cod_data_source_block           ch1ppx80_0m
_cod_depositor_comments
'Adding full bibliography for 7040891--7040897.cif.'
_cod_database_code               7040892
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              26328