Stepwise Formation of Tetra- and Hexanuclear Iridium and Rhodium Complexes Containing Oxalato Ligands
Han, Ying-Feng; Lin, Yue-Jian; Jia, Wei-Guo; Weng, Lin-Hong; Jin, Guo-Xin; Organometallics 26 (2007) 5848–; doi:10.1021/om700691u

data_4073865
_publ_section_title
;
 Stepwise Formation of Tetra- and Hexanuclear Iridium and Rhodium
 Complexes Containing Oxalato Ligands
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5848
_journal_paper_doi               10.1021/om700691u
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C72 H76 F12 Ir4 N8 O22 S4'
_chemical_formula_weight         2530.45
_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                 91.905(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.654(5)
_cell_length_b                   30.945(10)
_cell_length_c                   18.917(6)
_cell_measurement_reflns_used    897
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.720
_cell_measurement_theta_min      2.030
_cell_volume                     9744(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0741
_diffrn_reflns_av_sigmaI/netI    0.1209
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40809
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.26
_diffrn_standards_decay_%        5.31
_exptl_absorpt_coefficient_mu    5.620
_exptl_absorpt_correction_T_max  0.6620
_exptl_absorpt_correction_T_min  0.4861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4880
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.487
_refine_diff_density_min         -1.426
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1059
_refine_ls_number_reflns         17143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.118
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1005P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1666
_refine_ls_wR_factor_ref         0.1864
_reflns_number_gt                8219
_reflns_number_total             17143
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700691u-file003.cif
_cod_data_source_block           f70530b
_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               4073865