Cp*IrIII-Catalyzed Oxidative Coupling of Benzoic Acids with Alkynes
Frasco, Daniel A.; Lilly, Cassandra P.; Boyle, Paul D.; Ison, Elon A.; ACS Catalysis 3 (2013) 2421–; doi:10.1021/cs400656q

data_4508376
_publ_section_title
;
 Cp*IrIII-Catalyzed Oxidative Coupling of Benzoic Acids with Alkynes
;
_journal_issue                   10
_journal_name_full               'ACS Catalysis'
_journal_page_first              2421
_journal_paper_doi               10.1021/cs400656q
_journal_volume                  3
_journal_year                    2013
_chemical_formula_sum            'C16 H21 F6 Ir O5 S'
_chemical_formula_weight         631.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.080(4)
_cell_length_b                   14.954(7)
_cell_length_c                   15.588(7)
_cell_measurement_reflns_used    9829
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      2.60
_cell_volume                     2116.6(17)
_computing_cell_refinement       SAINT
_computing_data_collection       Apex2
_computing_data_reduction        SAINT
_computing_molecular_graphics    NRCVAX
_computing_publication_material  cif2tables.py
_computing_structure_refinement  XL
_computing_structure_solution    XS
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker-Nonius Kappa Axis X8 Apex2'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            86206
_diffrn_reflns_theta_full        37.86
_diffrn_reflns_theta_max         39.53
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    6.482
_exptl_absorpt_correction_T_max  0.6120
_exptl_absorpt_correction_T_min  0.3123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.263
_refine_diff_density_min         -2.938
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 5196 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.006(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         11850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0664
_reflns_number_gt                8704
_reflns_number_total             11850
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs400656q_si_003.cif
_cod_data_source_block           x12153
_cod_database_code               4508376