Versatile κ2,η2-CLigands Assembled at Iridium via [2+2] Oxidative Cyclization
Torres, Olga; Martín, Marta; Sola, Eduardo; Organometallics 29 (2010) 3201–; doi:10.1021/om100390m

data_4066308
_publ_section_title
;
 Versatile \k2,\h2-CLigands Assembled at Iridium via [2+2] Oxidative
 Cyclization
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3201
_journal_paper_doi               10.1021/om100390m
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C21 H33 Ir N2 O4 P, C H2 Cl2, B F4'
_chemical_formula_sum            'C22 H35 B Cl2 F4 Ir N2 O4 P'
_chemical_formula_weight         772.40
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.040(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.5507(19)
_cell_length_b                   8.8012(9)
_cell_length_c                   17.5506(18)
_cell_measurement_reflns_used    9030
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.21
_cell_volume                     2843.9(5)
_computing_cell_refinement       'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP program, SHELXTL v6.10, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.10,BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34371
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.87
_diffrn_reflns_theta_min         1.11
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.996
_exptl_absorpt_correction_T_max  0.492
_exptl_absorpt_correction_T_min  0.360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
  within SAINT+ package, v. 6.01.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.292
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         6996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0236P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0584
_reflns_number_gt                5375
_reflns_number_total             6996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100390m_si_001.cif
_cod_data_source_block           marta28a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4066308