Intra- and Intermolecular Hydroamination of Alkynes Catalyzed byortho-Metalated Iridium Complexes
Lai, Rung-Yi; Surekha, K.; Hayashi, Akito; Ozawa, Fumiyuki; Liu, Yi-Hong; Peng, Shie-Ming; Liu, Shiuh-Tzung; Organometallics 26 (2007) 1062–; doi:10.1021/om060965c

data_4072708
_publ_section_title
;
 Intra- and Intermolecular Hydroamination of Alkynes Catalyzed
 byortho-Metalated Iridium Complexes
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1062
_journal_paper_doi               10.1021/om060965c
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C35 H36 B Cl4 F4 Ir N P'
_chemical_formula_weight         922.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.025(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.140(3)
_cell_length_b                   13.6774(14)
_cell_length_c                   23.659(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      14.76
_cell_measurement_theta_min      9.58
_cell_volume                     3602.6(11)
_computing_cell_refinement       'Nonius CAD4'
_computing_data_collection       'Nonius CAD4'
_computing_data_reduction        'NRCSDP DATRD2'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_method       '\w--2\q 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0895
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5627
_diffrn_reflns_theta_full        23.97
_diffrn_reflns_theta_max         23.97
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        56
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.095
_exptl_absorpt_correction_T_max  0.3117
_exptl_absorpt_correction_T_min  0.2421
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.36
_refine_diff_density_max         1.958
_refine_diff_density_min         -1.674
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         5627
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+35.9172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1395
_reflns_number_gt                3784
_reflns_number_total             5627
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060965csi20061208_125025.cif
_cod_data_source_block           ic6229
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3602.7(11)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4072708