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_4114781
_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         'C21 H15 Ir3 Mo O11 '
_chemical_formula_sum            'C21 H15 Ir3 Mo O11'
_chemical_formula_weight         1115.94
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2001-04-13
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
Supplementary Material for JA0173829
;
_cell_angle_alpha                90
_cell_angle_beta                 91.84(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.523(4)
_cell_length_b                   19.434(3)
_cell_length_c                   15.469(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      15.9
_cell_measurement_theta_min      12.0
_cell_volume                     2560.9(14)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
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_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
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_diffrn_orient_matrix_UB_12      0.04820
_diffrn_orient_matrix_UB_13      -0.01295
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_diffrn_orient_matrix_UB_23      0.06309
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_diffrn_orient_matrix_UB_32      -0.01595
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_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.04896
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_diffrn_reflns_limit_l_min       -18
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_diffrn_standards_decay_%        15.98
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    16.012
_exptl_absorpt_correction_T_max  0.383
_exptl_absorpt_correction_T_min  0.142
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            orange
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_exptl_crystal_description       needle
_exptl_crystal_F_000             2008.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.22
_refine_diff_density_min         -2.51
_refine_ls_extinction_coef       0.00000042(1)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   1.901
_refine_ls_goodness_of_fit_ref   2.169
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
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_refine_ls_number_reflns         3229
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.0015
_refine_ls_shift/su_mean         0.0001
_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         0.0541
_refine_ls_wR_factor_ref         0.0513
_reflns_number_gt                3229
_reflns_number_total             4539
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            ja0173829_1.cif
_cod_data_source_block           7
_cod_original_cell_volume        2561(1)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C21 H15 Ir3 Mo O11 '
_cod_database_code               4114781