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_4065993
_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            'C84 H116 Ir4 N4 O18'
_chemical_formula_weight         2238.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.563(4)
_cell_angle_beta                 92.802(4)
_cell_angle_gamma                112.950(4)
_cell_formula_units_Z            1
_cell_length_a                   11.601(4)
_cell_length_b                   14.226(5)
_cell_length_c                   14.479(5)
_cell_measurement_reflns_used    6162
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.81
_cell_measurement_theta_min      2.44
_cell_volume                     2196.7(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      203(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0708
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11730
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        3.28
_exptl_absorpt_coefficient_mu    6.105
_exptl_absorpt_correction_T_max  0.5804
_exptl_absorpt_correction_T_min  0.4062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.549
_refine_diff_density_min         -2.143
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         8394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0412P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                6504
_reflns_number_total             8394
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1002396_si_001.cif
_cod_data_source_block           f91027a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_cell_volume        2196.6(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065993