Mixed-Metal Cluster Chemistry. 19. Crystallographic, Spectroscopic, Electrochemical, Spectroelectrochemical, and Theoretical Studies of Systematically Varied Tetrahedral Group 6-Iridium Clusters
Nigel T. Lucas; Jonathan P. Blitz; Simon Petrie; Robert Stranger; Mark G. Humphrey; Graham A. Heath; Vincent Otieno-Alego; Journal of the American Chemical Society 124 (2002) 5139–5153; doi:10.1021/ja0173829

data_4114783
_publ_contact_author_address
;
Department of Chemistry
Australian National University
Canberra ACT 0200
Australia
;
_publ_contact_author_email       ' Mark.Humphrey@anu.edu.au '
_publ_contact_author_fax         ' 61 2 6125 0760 '
_publ_contact_author_name        ' Mark G. Humphrey'
_publ_contact_author_phone       ' 61 2 6125 2927 '
_publ_section_title
;
 Mixed-Metal Cluster Chemistry. 19. Crystallographic, Spectroscopic,
 Electrochemical, Spectroelectrochemical, and Theoretical Studies of
 Systematically Varied Tetrahedral Group 6-Iridium Clusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5139
_journal_page_last               5153
_journal_paper_doi               10.1021/ja0173829
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         'C19 H16 Ir3 O10 P W '
_chemical_formula_sum            'C19 H16 Ir3 O10 P W'
_chemical_formula_weight         1195.81
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2001-04-14
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
?
;
_cell_angle_alpha                81.7838(5)
_cell_angle_beta                 72.8327(5)
_cell_angle_gamma                68.1183(8)
_cell_formula_units_Z            2
_cell_length_a                   9.2819(1)
_cell_length_b                   9.6886(1)
_cell_length_c                   14.9537(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    473.2
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     1191.46(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction
;
Denzo and Scalepak (Otwinowski & Minor, 1997)
;
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      200
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.11961
_diffrn_reflns_av_sigmaI/netI    0.070
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28946
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         3.14
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.684
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
gaussian (Coppens, 1970) implemented in maXus (1999)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.333
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1060.00
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.18
_refine_diff_density_max         6.07
_refine_diff_density_min         -5.56
_refine_ls_extinction_coef       0.00000037(4)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   1.367
_refine_ls_goodness_of_fit_ref   1.410
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     308
_refine_ls_number_reflns         6038
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0595
_refine_ls_wR_factor_ref         0.0570
_reflns_number_gt                6038
_reflns_number_total             6967
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            ja0173829_3.cif
_cod_data_source_block           13
_cod_original_cell_volume        1191.46(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C19 H16 Ir3 O10 P W '
_cod_database_code               4114783