Mixed-Metal Cluster Chemistry. 28. Core Enlargement of Tungsten-Iridium Clusters with Alkynyl, Ethyndiyl, and Butadiyndiyl Reagents
Gulliver T. Dalton; Lydie Viau; Susan M. Waterman; Mark G. Humphrey; Michael I. Bruce; Paul J. Low; Rachel L. Roberts; Anthony C. Willis; George A. Koutsantonis; Brian W. Skelton; Allan H. White; Inorganic Chemistry 44 (2005) 3261–3269; doi:10.1021/ic050040+

data_4327317
_publ_contact_author_address
;
Research School of Chemistry,
Australian National University,
Canberra, A. C. T. 0200, Australia
;
_publ_contact_author_email       ' willis@rsc.anu.edu.au '
_publ_contact_author_fax         ' 61 2 6125 0750 '
_publ_contact_author_name        ' Anthony C. Willis '
_publ_contact_author_phone       ' 61 2 6125 4109 '
_publ_section_title
;
 Mixed-Metal Cluster Chemistry. 28. Core Enlargement of Tungsten-Iridium
 Clusters with Alkynyl, Ethyndiyl, and Butadiyndiyl Reagents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3261
_journal_page_last               3269
_journal_paper_doi               10.1021/ic050040+
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C33 H25 Ir3 O10 W2 '
_chemical_formula_sum            'C33 H25 Ir3 O10 W2'
_chemical_formula_weight         1525.92
_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
_audit_creation_date             02-13-06
_audit_creation_method           CRYSTALS_ver_12-03-99
_audit_update_record
;
2002-06-14 - Report on C23 H25 Ir3 O10 W2
             by Anthony C. Willis
             for  Mark Humphrey and Gulliver T. Dalton
2002-06-14 - passes checkcif tests with minor warnings 
;
_cell_angle_alpha                95.2323(6)
_cell_angle_beta                 99.5846(6)
_cell_angle_gamma                100.5873(5)
_cell_formula_units_Z            2
_cell_length_a                   9.5204(1)
_cell_length_b                   10.8559(1)
_cell_length_c                   17.9731(3)
_cell_measurement_reflns_used    61580
_cell_measurement_temperature    200
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1786.18(4)
_computing_cell_refinement
;
 Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
 COLLECT (Nonius BV, 1997)
;
_computing_data_reduction
;
 Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics
;
teXsan (MSC, 1992-1997)
;
_computing_publication_material
;
 CRYSTALS (Watkin et al 2001)
;
_computing_structure_refinement
;
 CRYSTALS (Watkin et al 2001)
;
_computing_structure_solution
;
 SIR92 (Altomare et al, 1994)
;
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
;
Enraf Nonius Kappa CCD
;
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.08
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40961
_diffrn_reflns_theta_full        30.
_diffrn_reflns_theta_max         30.09
_diffrn_reflns_theta_min         4.16
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.604
_exptl_absorpt_correction_T_max  0.256
_exptl_absorpt_correction_T_min  0.043
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
gaussian integration (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            ' purple '
_exptl_crystal_density_diffrn    2.837
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             1347.926
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.75
_refine_diff_density_min         -1.53
_refine_ls_extinction_coef       7.4(15)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.0503
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7207
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.001114
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979,
 1.64    -.266     1.04   
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0350
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                7207
_reflns_number_total             10500
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            ic0500402Bsi20050111_065545_1.cif
_cod_data_source_block           gtd3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'triclinic ' changed to 'triclinic'
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 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C33 H25 Ir3 O10 W2 '
_cod_database_code               4327317