Acyl Protection Strategy for Synthesis of a Protic NHC Complex via N-Acyl Methanolysis†
Dobereiner, Graham E.; Chamberlin, Catherine A.; Schley, Nathan D.; Crabtree, Robert H.; Organometallics 29 (2010) 5728–; doi:10.1021/om100452g

data_4066414
_publ_section_title
;
 Acyl Protection Strategy for Synthesis of a Protic NHC Complex via N-Acyl
 Methanolysis&#x2020;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5728
_journal_paper_doi               10.1021/om100452g
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C27 H28 Cl Ir N2 O5 '
_chemical_formula_sum            'C27 H28 Cl Ir N2 O5'
_chemical_formula_weight         688.20
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.3027(19)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   24.6931(19)
_cell_length_b                   11.4909(9)
_cell_length_c                   17.7679(14)
_cell_measurement_reflns_used    15006
_cell_measurement_temperature    223.1
_cell_measurement_theta_max      27.7
_cell_measurement_theta_min      3.0
_cell_volume                     5037.5(7)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS97
_diffrn_detector_area_resol_mean 6.85
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku SCXmini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17065
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    5.463
_exptl_absorpt_correction_T_max  0.646
_exptl_absorpt_correction_T_min  0.309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2704.00
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.13
_refine_diff_density_min         -2.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5737
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0426P)^2^+8.1514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                4175
_reflns_number_total             5737
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om100452g_si_001.cif
_cod_data_source_block           (Benzoyl-NHC)Ir(cod)Cl
_cod_original_formula_sum        'C27 H28 Cl Ir N2 O5 '
_cod_database_code               4066414