The Si2H radical supported by two N-heterocyclic carbenes
Arz, Marius I.; Schnakenburg, Gregor; Meyer, Andreas; Schiemann, Olav; Filippou, Alexander C.; Chem. Sci. 7 (2016) 4973–; doi:10.1039/C6SC01569G

data_1543273
_publ_section_title
;
 The Si2H radical supported by two N-heterocyclic carbenes
;
_journal_issue                   8
_journal_name_full               'Chem. Sci.'
_journal_page_first              4973
_journal_paper_doi               10.1039/C6SC01569G
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C54 H73 N4 Si2'
_chemical_formula_sum            'C54 H73 N4 Si2'
_chemical_formula_weight         834.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-03-29 deposited with the CCDC.
2016-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.432(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9588(11)
_cell_length_b                   13.5352(9)
_cell_length_c                   18.2226(15)
_cell_measurement_reflns_used    3919
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.97
_cell_measurement_theta_min      2.71
_cell_volume                     2571.6(4)
_computing_cell_refinement       'STOE X-AREA, STOE&CIE, 2011'
_computing_data_collection       'STOE X-AREA, STOE&CIE, 2011'
_computing_data_reduction        'STOE X-RED, STOE&CIE, 2011'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
' 171 frames, detector distance = 100 mm, exposure time = 4min'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1649
_diffrn_reflns_av_unetI/netI     0.2106
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20621
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         2.712
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.9185
_exptl_absorpt_correction_T_min  0.6417
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XRed, STOE & CIE, 2011'
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             906
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.754
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         6197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.754
_refine_ls_R_factor_all          0.1885
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0929P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1721
_refine_ls_wR_factor_ref         0.2042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2130
_reflns_number_total             6197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc01569g2.cif
_cod_data_source_block           3756
_cod_depositor_comments          'Adding full bibliography for 1543273.cif.'
_cod_database_code               1543273
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              62786
_shelx_hkl_checksum              23943