Olefin Cyclopropanation Catalyzed by Iridium(III) Porphyrin Complexes
Anding, Bernie J.; Ellern, Arkady; Woo, L. Keith; Organometallics 31 (2012) 3628–; doi:10.1021/om300135f

data_4078251
_publ_section_title
;
 Olefin Cyclopropanation Catalyzed by Iridium(III) Porphyrin Complexes
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              3628
_journal_paper_doi               10.1021/om300135f
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C53 H49 Cl5 Ir N5'
_chemical_formula_weight         1125.42
_chemical_name_common            'Ir(TTP)(NMe3)Cl  (Compound #3)'
_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           'APEX2 v2010.3-0'
_cell_angle_alpha                90
_cell_angle_beta                 102.0610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0353(11)
_cell_length_b                   15.4171(13)
_cell_length_c                   24.578(2)
_cell_measurement_reflns_used    9556
_cell_measurement_temperature    173.(2)
_cell_measurement_theta_max      29.4732
_cell_measurement_theta_min      2.3625
_cell_volume                     4830.3(7)
_computing_cell_refinement       'SAINT V7.66A (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 Suite (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.66A (Bruker AXS, 2009)'
_computing_molecular_graphics    'XSHELL (Bruker AXS, 2007)'
_computing_publication_material  'APEX2 Suite (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  ' BRUKER APEX2 CCD Diffractometer'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            51968
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         29.50
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    3.083
_exptl_absorpt_correction_T_max  0.51
_exptl_absorpt_correction_T_min  0.32
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.219
_refine_diff_density_min         -1.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         13362
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+5.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0645
_reflns_number_gt                11836
_reflns_number_total             13362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300135f_si_002.cif
_cod_data_source_block           I
_cod_database_code               4078251