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_4327321
_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         ' C37 H25 Ir3 O13 W3 , C H2 Cl2'
_chemical_formula_sum            'C38 H27 Cl2 Ir3 O13 W3'
_chemical_formula_weight         1890.74
_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             04-09-09
_audit_creation_method           CRYSTALS_ver_12-03-99
_audit_update_record
;
2004-09-09 - Report on C38 H27 Cl2 Ir3 O13 W3
             by Anthony C. Willis
             for  Mark Humphrey and Lydie Viau
2004-09-09 - passes checkcif tests with minor warnings  
;
_cell_angle_alpha                103.8998(8)
_cell_angle_beta                 93.3532(10)
_cell_angle_gamma                95.1018(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3264(1)
_cell_length_b                   13.5767(2)
_cell_length_c                   15.6551(3)
_cell_measurement_reflns_used    36571
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     2114.86(6)
_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
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2003) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2003) 
;
_computing_structure_solution
; 
 SIR92 (Altomare et al, 1994) 
;
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
; 
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  0.09
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            52181
_diffrn_reflns_theta_full        27.497
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.690
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.716
_exptl_absorpt_correction_T_max  0.514
_exptl_absorpt_correction_T_min  0.121
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            ' black '
_exptl_crystal_density_diffrn    2.969
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.14
_refine_diff_density_min         -2.86
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9797
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         7384
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.001525
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 1.87 0.307 1.47 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0413
_refine_ls_wR_factor_gt          0.0390
_refine_ls_wR_factor_ref         0.0390
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                7384
_reflns_number_total             9708
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic0500402Bsi20050111_065545_5.cif
_cod_data_source_block           mgh042
_cod_original_cell_volume        2114.86(5)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C38 H27 Cl2 Ir3 O13 W3 '
_cod_database_code               4327321