Annulation of an Iridabenzene through Formal Cycloaddition Reactions with Organonitriles
Dalebrook, Andrew F.; Wright, L. James; Organometallics 28 (2009) 5536–; doi:10.1021/om900581h

data_4070042
_publ_section_title
;
 Annulation of an Iridabenzene through Formal Cycloaddition Reactions with
 Organonitriles
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              5536
_journal_paper_doi               10.1021/om900581h
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C58 H51 Cl2 F12 Ir N2 P4 S'
_chemical_formula_weight         1423.12
_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
_audit_update_record
;
2009-07-01 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.7850(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5325(2)
_cell_length_b                   34.4058(4)
_cell_length_c                   15.2538(2)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      51.994
_cell_measurement_theta_min      4.759
_cell_volume                     6414.23(15)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Ortep-III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       'Area detector \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  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            71236
_diffrn_reflns_theta_full        27.82
_diffrn_reflns_theta_max         27.82
_diffrn_reflns_theta_min         1.18
_diffrn_standards_decay_%        <2%
_exptl_absorpt_coefficient_mu    2.369
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         1.290
_refine_diff_density_min         -2.921
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         15192
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+34.8007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                12522
_reflns_number_total             15192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900581h_si_002.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4070042