Synthesis and Reactivity of Cationic Iridium Aminocarbenes Derived from Terminal Alkynes and 2-Aminopyridines
Kumaran, Elumalai; How, Kai Tong Sonia; Ganguly, Rakesh; Li, Yongxin; Leong, Weng Kee; Organometallics 32 (2013) 4149–; doi:10.1021/om400326c

data_4081000
_publ_section_title
;
 Synthesis and Reactivity of Cationic Iridium Aminocarbenes Derived from
 Terminal Alkynes and 2-Aminopyridines
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4149
_journal_paper_doi               10.1021/om400326c
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C25.75 H29.5 Br Cl5.5 Ir N2 O'
_chemical_formula_weight         850.10
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.5970(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.4513(2)
_cell_length_b                   22.3781(5)
_cell_length_c                   29.0848(7)
_cell_measurement_reflns_used    7049
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      26.70
_cell_measurement_theta_min      2.30
_cell_volume                     6145.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0937
_diffrn_reflns_av_sigmaI/netI    0.1073
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            64543
_diffrn_reflns_theta_full        28.66
_diffrn_reflns_theta_max         28.66
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    6.147
_exptl_absorpt_correction_T_max  0.5785
_exptl_absorpt_correction_T_min  0.3728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3292
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.850
_refine_diff_density_min         -2.025
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         15631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1296
_reflns_number_gt                9624
_reflns_number_total             15631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400326c_si_001.cif
_cod_data_source_block           lwk47s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C25.75 H29.50 Br Cl5.50 Ir N2 O'
_cod_database_code               4081000