New 13-vertex metallacarborane sandwich compounds; synthetic and structural studies
Ellis, David; McIntosh, Ruaraidh D.; Esquirolea, Susana; Viñas, Clara; Rosair, Georgina M.; Teixidor, Francesc; Welch, Alan J.; Dalton Transactions  (2008) 1009–1017; doi:10.1039/b716169g

data_7003441
_publ_section_title
;
 New 13-vertex metallacarborane sandwich compounds; synthetic and
 structural studies
;
_journal_issue                   8
_journal_name_full               'Dalton Transactions'
_journal_page_first              1009
_journal_page_last               1017
_journal_paper_doi               10.1039/b716169g
_journal_year                    2008
_chemical_formula_sum            'C16 H49 B20 Fe K O6.5'
_chemical_formula_weight         656.70
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.939(9)
_cell_angle_beta                 105.521(9)
_cell_angle_gamma                94.770(9)
_cell_formula_units_Z            2
_cell_length_a                   11.1550(18)
_cell_length_b                   11.4338(19)
_cell_length_c                   13.759(2)
_cell_measurement_reflns_used    3773
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     1655.9(5)
_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 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0719
_diffrn_reflns_av_sigmaI/netI    0.0859
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25741
_diffrn_reflns_theta_full        24.80
_diffrn_reflns_theta_max         24.80
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            pale
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.790
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         5532
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.1288
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0942P)^2^+5.9631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1837
_refine_ls_wR_factor_ref         0.2178
_reflns_number_gt                3638
_reflns_number_total             5532
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b716169g.txt
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1656.0(5)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C16 H49 B20 Fe K O6.50'
_cod_database_code               7003441