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_7043061
_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         'C40 H51 Li N2 O7 W'
_chemical_formula_sum            'C40 H51 Li N2 O7 W'
_chemical_formula_weight         862.61
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-15
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2016-11-08 deposited with the CCDC.
2017-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.4081(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.86235(11)
_cell_length_b                   18.91698(18)
_cell_length_c                   19.27237(18)
_cell_measurement_reflns_used    54851
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      31.9580
_cell_measurement_theta_min      2.1090
_cell_volume                     3960.04(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -4.00  94.00   1.00    4.00    --   24.96  77.00 150.00   98
  2  \w      6.00  93.00   1.00    4.00    --   24.96  57.00 -90.00   87
  3  \w    -43.00  43.00   1.00    4.00    --   24.96 -57.00-150.00   86
  4  \w    -43.00  43.00   1.00    4.00    --   24.96 -57.00 120.00   86
  5  \w    -47.00  63.00   1.00    4.00    --   24.96 -19.00 -90.00  110
  6  \w     -4.00  94.00   1.00    4.00    --   24.96  77.00 -30.00   98
  7  \w      6.00  93.00   1.00    4.00    --   24.96  57.00  90.00   87
  8  \w    -44.00  54.00   1.00    4.00    --   24.96 -77.00  60.00   98
  9  \w    -20.00  65.00   1.00    4.00    --   24.96 -99.00-180.00   85
 10  \w     10.00  89.00   1.00    4.00    --   24.96-139.00  20.61   79
 11  \w    -97.00 -16.00   1.00    4.00    --  -23.50 153.00 -28.14   81
 12  \w    -94.00 -31.00   1.00    4.00    --  -23.50 -38.00  60.00   63
 13  \w     -4.00  94.00   1.00    4.00    --   24.96  77.00  30.00   98
 14  \w      7.00  85.00   1.00    4.00    --   24.96-133.00 -79.43   78
 15  \w     -4.00  94.00   1.00    4.00    --   24.96  77.00-150.00   98
 16  \w    -47.00  63.00   1.00    4.00    --   24.96 -19.00  90.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0311421000
_diffrn_orient_matrix_UB_12      0.0322041000
_diffrn_orient_matrix_UB_13      0.0070235000
_diffrn_orient_matrix_UB_21      -0.0572110000
_diffrn_orient_matrix_UB_22      0.0168023000
_diffrn_orient_matrix_UB_23      0.0062799000
_diffrn_orient_matrix_UB_31      0.0044576000
_diffrn_orient_matrix_UB_32      -0.0093246000
_diffrn_orient_matrix_UB_33      0.0355785000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            137501
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.080
_diffrn_reflns_theta_min         1.508
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.966
_exptl_absorpt_correction_T_max  0.736
_exptl_absorpt_correction_T_min  0.511
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       block
_exptl_crystal_F_000             1752.0
_exptl_crystal_recrystallization_method
'disordered from C37 to C40. Inside the disordred part ADP's were constrained to be same pairwise, equivalent bond length were restrained to be same'
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.126
_refine_diff_density_max         1.262
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         11634
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+3.0934P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10239
_reflns_number_total             11634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01199g2.cif
_cod_data_source_block           raj01
_cod_database_code               7043061
_chemical_oxdiff_formula         'C132 H216 N48 O20 W4 Li1 '
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_date_sample_data_collection 2016-07-14
_olex2_exptl_crystal_mounting_method mounted
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.473
_oxdiff_exptl_absorpt_empirical_full_min 0.673
_shelx_res_checksum              74651
_shelxl_version_number           2013-2