Unusual 9 →10 Rearrangement of the Substituted Cage Carbon in the Ferratricarbollide Series. Synthesis of the Isomeric Complexes [2-ν^5^-(C~5~H~5~)-10-X-closo-2,1,7,10-FeC~3~B~8~H~10~] (where X = H~2~N, MeHN, Me~2~N and Bu^t^HN)
Bohumír Grüner; Ari Lehtonen; Raikko Kivekäs; Reijo Sillanpää; Josef Holub; Francesc Teixidor; Clara Viñas; Bohumil Štíbr; Inorganic Chemistry 39 (2000) 2577–2580; doi:10.1021/ic991375s

data_4321044
_publ_contact_author
;    Dr Bohumil Stibr, DSc
     Institute of Inorganic Chemistry
     Academy of Sciences of the Czech Republic
     25056 Rez
     Czech Republic
;
_publ_contact_author_email       stibr@iic.cas.cz
_publ_contact_author_fax         +4202-20940161
_publ_contact_author_phone       +4202-66173106
_publ_section_title
;
 Unusual 9 \\rightarrow 10 Rearrangement of the Substituted Cage Carbon in
 the Ferratricarbollide Series. Synthesis of the Isomeric Complexes
 [2-\n^5^-(C~5~H~5~)-10-X-closo-2,1,7,10-FeC~3~B~8~H~10~] (where X =
 H~2~N, MeHN, Me~2~N and Bu^t^HN)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2577
_journal_page_last               2580
_journal_paper_doi               10.1021/ic991375s
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         'C12 H25 B8 Fe N'
_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 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.37(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.149(4)
_cell_length_b                   6.501(4)
_cell_length_c                   19.421(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      9.94
_cell_measurement_theta_min      6.21
_cell_volume                     1657.3(12)
_computing_cell_refinement
;
MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 
1993)
;
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 
1993)
;
_computing_data_reduction
;
Texsan Process (Molecular Structure Corporation, 1993)
;
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.863
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       \w--2\q
_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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5045
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.10
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  0.8772
_exptl_absorpt_correction_T_min  0.6883
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North, Phillips & Mathews 1968'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.0039(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2763
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+2.5050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                2371
_reflns_number_total             2763
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991375s.cif
_cod_data_source_block           compound_3d
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+2.5050P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+2.5050P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321044