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_4321413
_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_sum            'C64 H64 Cl4 F3 Ir2 N8 O10'
_chemical_formula_weight         1688.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.225(2)
_cell_length_b                   24.799(7)
_cell_length_c                   22.912(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      16.52
_cell_measurement_theta_min      14.08
_cell_volume                     13196(4)
_computing_cell_refinement       'CAD4 V5'
_computing_data_collection       'CAD4 V5'
_computing_data_reduction        XCAD4
_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      173(2)
_diffrn_measurement_device       'Nonius CAD4'
_diffrn_measurement_method       'Omega two-theta 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  0.0569
_diffrn_reflns_av_sigmaI/netI    0.1074
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            10029
_diffrn_reflns_theta_max         22.39
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    4.263
_exptl_absorpt_correction_T_max  0.398
_exptl_absorpt_correction_T_min  0.267
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       tablet
_exptl_crystal_F_000             6664
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.373
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.017
_refine_ls_goodness_of_fit_obs   1.145
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         8482
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.016
_refine_ls_restrained_S_obs      1.143
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_obs          0.0425
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+42.8116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1158
_refine_ls_wR_factor_obs         0.0923
_reflns_number_observed          4632
_reflns_number_total             8482
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000527c_1.cif
_cod_data_source_block           cmpd_1
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'psiscan' changed
to 'psi-scan' 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 'none' 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^)+(0.0434P)^2^+42.8116P] 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^)+(0.0434P)^2^+42.8116P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        13196.3(43)
_cod_database_code               4321413