A 10-Vertex Iron−Dicarbollide System Formed by Insertion of {Fe(CO)4} into 8-Vertex [closo-1-CB7H8]−: Synthesis and Reactivity Studies
Franken, Andreas; McGrath, Thomas D.; Stone, F. Gordon A.; Organometallics 27 (2008) 908–; doi:10.1021/om700865s

data_4070604
_publ_section_title
;
 A 10-Vertex Iron&#x2212;Dicarbollide System Formed by Insertion of
 {Fe(CO)4} into 8-Vertex [closo-1-CB7H8]&#x2212;: Synthesis and Reactivity
 Studies
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              908
_journal_paper_doi               10.1021/om700865s
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C31.5 H52 B7 Fe N2 O P'
_chemical_formula_weight         637.24
_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                 90.564(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.040(3)
_cell_length_b                   15.018(3)
_cell_length_c                   18.379(4)
_cell_measurement_reflns_used    2446
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      20.37
_cell_measurement_theta_min      2.34
_cell_volume                     3599.1(13)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2003)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2003)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2003)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 2001)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'Bruker SHELXTL (Bruker, 2001)'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker-Nonius X8 APEX 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  0.1194
_diffrn_reflns_av_sigmaI/netI    0.1164
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43480
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.77
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    0.490
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         8387
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0452P)^2^+1.2093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1339
_reflns_number_gt                4636
_reflns_number_total             8387
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700865s-file001.cif
_cod_data_source_block           10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3599.1(14)
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_original_formula_sum        'C31.50 H52 B7 Fe N2 O P'
_cod_database_code               4070604