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_4321415
_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            'C53 H62 Ir2 N4 O4'
_chemical_formula_weight         1203.47
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.16(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.195(3)
_cell_length_b                   27.420(3)
_cell_length_c                   18.306(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      16.53
_cell_measurement_theta_min      14.07
_cell_volume                     4615(2)
_computing_cell_refinement       'CAD4 V5 (Nonius, 1989)'
_computing_data_collection       'CAD4 V5 (Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms, 1993)'
_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-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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6432
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.812
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.054
_refine_ls_goodness_of_fit_obs   1.093
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         5992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_restrained_S_obs      1.093
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_obs          0.0296
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+10.8443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0773
_refine_ls_wR_factor_obs         0.0716
_reflns_number_observed          4893
_reflns_number_total             5993
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000527c_3.cif
_cod_data_source_block           cmpd_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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^)+(0.0338P)^2^+10.8443P] 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^)+(0.0338P)^2^+10.8443P] 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        4615.4(20)
_cod_database_code               4321415