Imidazolium ylides from a conjugate addition-proton transfer route and their cycloaddition reactions
Raymond C. F. Jones; James N. Iley; Maria Sanchis-Amat; Xiaohui Zhang; Vickie McKee; Simon J. Coles; Thomas Gelbrich; Chem.Commun. 47 (2011) 7965–; doi:10.1039/c1cc12255j

data_7106640
_publ_section_title
;
 Imidazolium ylides from a conjugate addition-proton transfer route and
 their cycloaddition reactions
;
_journal_name_full               Chem.Commun.
_journal_page_first              7965
_journal_paper_doi               10.1039/c1cc12255j
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C21 H25 N3 O6'
_chemical_formula_weight         415.44
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.18(3)
_cell_angle_beta                 108.98(3)
_cell_angle_gamma                90.44(3)
_cell_formula_units_Z            4
_cell_length_a                   11.331(2)
_cell_length_b                   13.023(3)
_cell_length_c                   15.005(3)
_cell_measurement_reflns_used    21725
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.82
_cell_measurement_theta_min      1.00
_cell_volume                     2055.8(9)
_computing_cell_refinement       'DENZO, COLLECT'
_computing_data_reduction        'DENZO, COLLECT'
_computing_molecular_graphics    'CAMERON (Watkin, Pearce 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Nonius KappaCCD Area Detector'
_diffrn_measurement_method       '\f and \w scans to fill Ewald Sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_sigmaI/netI    0.1097
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7560
_diffrn_reflns_theta_full        20.76
_diffrn_reflns_theta_max         20.76
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.9980
_exptl_absorpt_correction_T_min  0.9901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.020(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         4048
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1437
_refine_ls_R_factor_gt           0.1033
_refine_ls_shift/su_max          0.094
_refine_ls_shift/su_mean         0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1927P)^2^+2.7954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2628
_refine_ls_wR_factor_ref         0.3028
_reflns_number_gt                2645
_reflns_number_total             4048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc12255j.txt
_cod_data_source_block           01src383
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        2055.7(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7106640