Cleavage of C−H Bonds for Building Tetranuclear Half-Sandwich Iridium Macrocycles with Ortho-Metalated Spacers
Yu, Wei-Bin; Han, Ying-Feng; Lin, Yue-Jian; Jin, Guo-Xin; Organometallics 29 (2010) 2827–; doi:10.1021/om1002396

data_4065989
_publ_section_title
;
 Cleavage of C&#x2212;H Bonds for Building Tetranuclear Half-Sandwich
 Iridium Macrocycles with Ortho-Metalated Spacers
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2827
_journal_paper_doi               10.1021/om1002396
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C66 H92 Ir4 N4 O16'
_chemical_formula_weight         1966.24
_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                 110.514(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.306(11)
_cell_length_b                   22.39(2)
_cell_length_c                   14.133(14)
_cell_measurement_reflns_used    718
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.001
_cell_measurement_theta_min      2.196
_cell_volume                     3351(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1099
_diffrn_reflns_av_sigmaI/netI    0.1841
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13739
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        7.14
_exptl_absorpt_coefficient_mu    7.987
_exptl_absorpt_correction_T_max  0.6909
_exptl_absorpt_correction_T_min  0.4474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.949
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.946
_refine_diff_density_min         -2.092
_refine_diff_density_rms         0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.806
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         5910
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.806
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                2954
_reflns_number_total             5910
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1002396_si_001.cif
_cod_data_source_block           f81015c
_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 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4065989