Addition of Amines to a Carbonyl Ligand: Syntheses, Characterization, and Reactivities of Iridium(III) Porphyrin Carbamoyl Complexes
Dairo, Taiwo O.; Ellern, Arkady; Angelici, Robert J.; Woo, L. Keith; Organometallics 33 (2014) 2266–; doi:10.1021/om500189a

data_4083055
_publ_section_title
;
 Addition of Amines to a Carbonyl Ligand: Syntheses, Characterization, and
 Reactivities of Iridium(III) Porphyrin Carbamoyl Complexes
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2266
_journal_paper_doi               10.1021/om500189a
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C72 H74 Ir N7 O4'
_chemical_formula_weight         1293.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_cell_angle_alpha                77.200(5)
_cell_angle_beta                 86.527(5)
_cell_angle_gamma                81.073(5)
_cell_formula_units_Z            2
_cell_length_a                   9.833(3)
_cell_length_b                   16.673(5)
_cell_length_c                   20.164(7)
_cell_measurement_temperature    173.(2)
_cell_volume                     3183.4(18)
_computing_cell_refinement       'SAINT V7.66A (Bruker AXS, 2013)'
_computing_data_collection       'APEX2 Suite (Bruker AXS, 2013)'
_computing_data_reduction        'SAINT V7.66A (Bruker AXS, 2013)'
_computing_molecular_graphics    'XSHELL (Bruker AXS, 2007)'
_computing_publication_material  'APEX2 Suite (Bruker AXS, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173.(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ' full spere \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0805
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31176
_diffrn_reflns_theta_full        27.72
_diffrn_reflns_theta_max         27.72
_diffrn_reflns_theta_min         1.27
_diffrn_source                   'X-ray tuve'
_diffrn_source_type              'Sealed tube'
_exptl_absorpt_coefficient_mu    2.151
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2013)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.262
_refine_diff_density_min         -2.513
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         14716
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+4.5185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1463
_reflns_number_gt                11982
_reflns_number_total             14716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500189a_si_002.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 4083055--4083056.cif.'
_cod_database_code               4083055