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_4066415
_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         'C40 H43 Cl4 F6 Ir N2 O4 P2 '
_chemical_formula_sum            'C40 H43 Cl4 F6 Ir N2 O4 P2'
_chemical_formula_weight         1125.76
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                81.933(5)
_cell_angle_beta                 82.010(5)
_cell_angle_gamma                81.307(5)
_cell_formula_units_Z            2
_cell_length_a                   10.244(2)
_cell_length_b                   11.162(3)
_cell_length_c                   19.742(4)
_cell_measurement_reflns_used    18221
_cell_measurement_temperature    223.1
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      3.1
_cell_volume                     2193.3(9)
_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    SIR92
_diffrn_detector_area_resol_mean 6.85
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.055
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21073
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    3.436
_exptl_absorpt_correction_T_max  0.709
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1116.00
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.25
_refine_diff_density_min         -0.93
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     537
_refine_ls_number_reflns         9912
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0473P)^2^+0.3481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                7938
_reflns_number_total             9912
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om100452g_si_001.cif
_cod_data_source_block           '[(H-NHC)Ir(cod)PPh3]PF6'
_cod_original_cell_volume        2193.4(8)
_cod_original_formula_sum        'C40 H43 Cl4 F6 Ir N2 O4 P2 '
_cod_database_code               4066415