Formation, Stability, and Structures of Borenium and Boronium Cations Derived from Pentamethylazaferrocene‒Boranes by Hydride or Chloride Abstraction Reactions
Bentivegna, BriAnne; Mariani, Christine I.; Smith, Jason R.; Ma, Shuhua; Rheingold, Arnold L.; Brunker, Tim J.; Organometallics 33 (2014) 2820–; doi:10.1021/om500348u

data_4083365
_publ_section_title
;
 Formation, Stability, and Structures of Borenium and Boronium Cations
 Derived from Pentamethylazaferrocene--Boranes by Hydride or Chloride
 Abstraction Reactions
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2820
_journal_paper_doi               10.1021/om500348u
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C53 H42 B2 Cl2 F20 Fe2 N2'
_chemical_formula_weight         1291.11
_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                99.1030(10)
_cell_angle_beta                 90.7050(10)
_cell_angle_gamma                118.8660(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2305(8)
_cell_length_b                   13.6723(8)
_cell_length_c                   16.9454(16)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.43
_cell_measurement_theta_min      2.30
_cell_volume                     2636.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33356
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.48
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  0.8148
_exptl_absorpt_correction_T_min  0.7351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.28
_platon_squeeze_details
; 
 SQUEEZE (PLATON, A. Spek) was used to treat diffuse solvent 
 contributions.  Total electron count found = 81/unit cell.  Calculated for
 2 CH2Cl2 (the re'xtal solvent) = 84/unit cell.  The intensive
 properties (density, F(000), etc.) reflect these contributions.  
;
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         9764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0400P)^2^+1.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0857
_reflns_number_gt                8582
_reflns_number_total             9764
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500348u_si_002.cif
_cod_data_source_block           towson07
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4083363--4083368.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4083365