An N-Heterocyclic Carbene as a Bidentate Hemilabile Ligand: A Synchrotron X-ray Diffraction and Density Functional Theory Study
Morris Bullock; Vladimir K. Dioumaev; James A. Franz; Jonathan Hanson; David J. Szalda; Chemical communications (Cambridge, England)  (2003) –; doi:10.1039/b303762b

data_7103761
_publ_section_title
;
An N-Heterocyclic Carbene as a Bidentate Hemilabile
Ligand:  A Synchrotron X-ray Diffraction and Density Functional Theory
Study
;
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/b303762b
_journal_year                    2003
_chemical_formula_moiety
;
'( C28 H29 N2 O2 W ), ( C24 F20 B ), ( C3.5 H4 )' 
;
_chemical_formula_sum            'C55.5 H33 B F20 N2 O2 W'
_chemical_formula_weight         1334.50
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.87(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.262(4)
_cell_length_b                   17.725(4)
_cell_length_c                   17.657(4)
_cell_measurement_temperature    150(2)
_cell_volume                     5226.6(18)
_computing_cell_refinement
;
average of cell contants determined on each image plate
;
_computing_data_collection
;
see M.J. Gray etal for a description of data collection at beamline x7b
;
_computing_data_reduction        'DENZO, SCALEPACK (Otwinowski)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.761
_diffrn_measured_fraction_theta_max 0.761
_diffrn_measurement_device_type  Huber
_diffrn_measurement_method       'mar dectector'
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source
'National Synchrotron Light Source beamline x7b'
_diffrn_radiation_wavelength     0.90350
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4800
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    2.327
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2620
_exptl_crystal_size_max          .100
_exptl_crystal_size_mid          .050
_exptl_crystal_size_min          .010
_refine_diff_density_max         2.775
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         4800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.447
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0862P)^2^+53.9393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1540
_reflns_number_gt                4654
_reflns_number_total             4800
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303762b.txt
_cod_data_source_block           wvladfst
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C55.50 H33 B F20 N2 O2 W'
_cod_database_code               7103761