A Series of the Twelve-Vertex Ferratricarbollides [2-(η^5^-C~5~H~5~)-9-X-closo-2,1,7,9-FeC~3~B~8~H~10~] where X = H~2~N, MeHN,Me~2~N,Bu^t^HN, and Bu^t^(Me)N. A Highly Stable Metallatricarbaborane System with Amine Functions in the Para Position to the Metal Center
Josef Holub; Bohumír Grüner; Ivana Císařová; Jiří Fusek; Zbyněk Plzák; Francesc Teixidor; Clara Viñas; Bohumil Štíbr; Inorganic Chemistry 38 (1999) 2775–2780; doi:10.1021/ic981400e

data_4322079
_publ_contact_author_address
; 
Institute of Inorganic Chemistry Academy of Science
of Czech Republic 250 68 \<Re\<z Czech Republic 
;
_publ_contact_author_email       stibr@uachr.iic.cas.cz
_publ_contact_author_fax         420220941502
_publ_contact_author_name        'Ing. Bohumil \<St\'ibr'
_publ_section_title
;
 A Series of the Twelve-Vertex Ferratricarbollides
 [2-(\h^5^-C~5~H~5~)-9-X-closo-2,1,7,9-FeC~3~B~8~H~10~] where X = H~2~N,
 MeHN,Me~2~N,Bu^t^HN, and Bu^t^(Me)N. A Highly Stable
 Metallatricarbaborane System with Amine Functions in the Para Position to
 the Metal Center
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2775
_journal_page_last               2780
_journal_paper_doi               10.1021/ic981400e
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C12 H25 B8 Fe N'
_chemical_formula_weight         325.66
_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                 112.543(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8353(4)
_cell_length_b                   16.7280(10)
_cell_length_c                   12.2105(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      13.5
_cell_volume                     1666.78(18)
_computing_cell_refinement       'Cad4 Version 5.0'
_computing_data_collection       'CAD4 Version 5.0'
_computing_data_reduction        'JANA96 (Petricek, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  CAD4-MACHIII
_diffrn_measurement_method       'theta-2theta scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4486
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.892
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'JANA96 (Petricek,1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         2935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+0.5625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0872
_reflns_number_gt                2557
_reflns_number_total             2935
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic981400e.cif
_cod_data_source_block           2c
_cod_database_code               4322079