Synthesis and Structures of 1′,2′,3′,4′,5′-Pentamethylazaferrocene Complexes with Lewis Acidic Boranes
Brunker, Tim J.; Roembke, Benjamin T.; Golen, James A.; Rheingold, Arnold L.; Organometallics 30 (2011) 2272–; doi:10.1021/om200053p

data_4064338
_publ_section_title
;
 Synthesis and Structures of
 1&#x2032;,2&#x2032;,3&#x2032;,4&#x2032;,5&#x2032;-Pentamethylazaferrocene
 Complexes with Lewis Acidic Boranes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2272
_journal_paper_doi               10.1021/om200053p
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C14 H22 B Fe N'
_chemical_formula_sum            'C14 H22 B Fe N'
_chemical_formula_weight         270.99
_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                89.936(2)
_cell_angle_beta                 86.745(2)
_cell_angle_gamma                89.897(2)
_cell_formula_units_Z            20
_cell_length_a                   15.2204(17)
_cell_length_b                   15.4221(18)
_cell_length_c                   30.354(3)
_cell_measurement_reflns_used    9118
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.36
_cell_volume                     7113.5(13)
_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, 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.885
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            80946
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.15
_diffrn_reflns_theta_min         0.67
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  0.9499
_exptl_absorpt_correction_T_min  0.8193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1582
_refine_ls_number_reflns         30862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+3.6119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                25949
_reflns_number_total             30862
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om200053p_si_002.cif
_cod_data_source_block           towson02
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        7113.5(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064338