The Conformations of 13-Vertex ML~2~C~2~B~10~ Metallacarboranes: Experimental and Computational Studies
Kelly J. Dalby; David Ellis; Stefan Erhardt; Ruaraidh D. McIntosh; Stuart A. Macgregor; Karen Rae; Georgina M. Rosair; Volker Settels; Alan J. Welch; Bruce E. Hodson; Thomas D. McGrath; F. Gordon A. Stone; Journal of the American Chemical Society 129 (2007) 3302–3314; doi:10.1021/ja067698m

data_4109174
_publ_contact_author
;
        Prof Alan Welch
        Department of Chemistry
        Heriot-Watt University
        Edinburgh EH14 4AS
;
_publ_contact_author_email       A.J.Welch@hw.ac.uk
_publ_contact_author_fax         '0131 451 3180'
_publ_contact_author_phone       '0131 451-3217'
_publ_section_title
;
 The Conformations of 13-Vertex ML~2~C~2~B~10~ Metallacarboranes:
 Experimental and Computational Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3302
_journal_page_last               3314
_journal_paper_doi               10.1021/ja067698m
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C18 H34 B10 P2 Pt'
_chemical_formula_sum            'C18 H34 B10 P2 Pt'
_chemical_formula_weight         615.58
_chemical_name_systematic
; 
 ? 
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.028(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6694(9)
_cell_length_b                   10.5522(7)
_cell_length_c                   17.3895(12)
_cell_measurement_reflns_used    6950
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.22
_cell_measurement_theta_min      3.60
_cell_volume                     2470.0(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34349
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.22
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.816
_exptl_absorpt_correction_T_max  0.498
_exptl_absorpt_correction_T_min  0.315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick, 2002) SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.087
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         9430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0156
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0390
_refine_ls_wR_factor_ref         0.0397
_reflns_number_gt                8651
_reflns_number_total             9430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067698msi20070131_125137_2.cif
_cod_data_source_block           kr1cmpd3
_cod_database_code               4109174