A Reliable Method of Preparation of Diiridium Paddlewheel Complexes: Structures of the First Compounds with Ir25+ Cores
F. Albert Cotton; Chun Lin; Carlos A. Murillo; Inorganic Chemistry 39 (2000) 4574–4578; doi:10.1021/ic000527c

data_4321414
_publ_section_title
;
 A Reliable Method of Preparation of Diiridium Paddlewheel Complexes:
 Structures of the First Compounds with Ir25+ Cores
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4574
_journal_page_last               4578
_journal_paper_doi               10.1021/ic000527c
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         Ir2(p-Clform)4(O2CCF3).2CH2Cl2
_chemical_formula_sum            'C55 H38 Cl10 F3 Ir2 N8 O2'
_chemical_formula_weight         1638.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.51(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.107(4)
_cell_length_b                   12.510(2)
_cell_length_c                   16.406(3)
_cell_measurement_reflns_used    229
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.0
_cell_volume                     2895.2(11)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    'XP (Siemens, 1990)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10434
_diffrn_reflns_theta_max         22.57
_diffrn_reflns_theta_min         2.48
_diffrn_standards_number         'None (area detector data)'
_exptl_absorpt_coefficient_mu    5.113
_exptl_absorpt_correction_T_max  0.608
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1582
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.779
_refine_diff_density_min         -2.008
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.162
_refine_ls_goodness_of_fit_obs   1.152
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3741
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.193
_refine_ls_restrained_S_obs      1.150
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_obs          0.0631
_refine_ls_shift/esd_max         -0.016
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+65.2294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1596
_refine_ls_wR_factor_obs         0.1364
_reflns_number_observed          3004
_reflns_number_total             3768
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000527c_2.cif
_cod_data_source_block           cmpd_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+65.2294P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+65.2294P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321414