Normal-to-Abnormal Rearrangement of an N-Heterocyclic Carbene with a Silylene Transition Metal Complex
Ghadwal, Rajendra S.; Rottschaefer, Dennis; Andrada, Diego Marcelo; Frenking, G.; Schürmann, Christian J.; Stammler, Georg; Dalton Trans.  (2017) –; doi:10.1039/C7DT01199G

data_7043064
_publ_section_title
;
 Normal-to-Abnormal Rearrangement of an N-Heterocyclic Carbene with a
 Silylene Transition Metal Complex
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01199G
_journal_year                    2017
_chemical_formula_moiety         'C58 H72 Cl4 N4 O4 Si2 W, C5 H5 N, C H2 Cl2'
_chemical_formula_sum            'C64 H79 Cl6 N5 O4 Si2 W'
_chemical_formula_weight         1435.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-11-03 deposited with the CCDC.
2017-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.35(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.696(2)
_cell_length_b                   16.539(3)
_cell_length_c                   16.499(3)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.471
_cell_measurement_theta_min      2.301
_cell_volume                     3370.8(11)
_computing_cell_refinement       'SAINT V8.30C'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V8.30C'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
'SHELXT (G.M.Sheldrick,Acta Cryst.(2015)A71,3-8)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57844
_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         27.487
_diffrn_reflns_theta_min         1.231
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    2.035
_exptl_absorpt_correction_T_max  0.2616
_exptl_absorpt_correction_T_min  0.2002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       needle
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.371
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 7215 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0060(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         15424
_refine_ls_number_restraints     377
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0185
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+1.0206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0442
_refine_ls_wR_factor_ref         0.0447
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                14942
_reflns_number_total             15424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01199g2.cif
_cod_data_source_block           Compound_4W
_cod_database_code               7043064
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.519
_shelx_estimated_absorpt_t_max   0.864
_shelx_res_checksum              57418