Synthesis and Structural Characterization of the Diborylated Organometallics 1,3-Bis(dibromoboryl)-1′,2′,3′,4′,5′-(pentamethyl)ferrocene and 1,3-Bis(dibromoboryl)cymantrene
Eckensberger, U. David; Kunz, Kerstin; Bolte, Michael; Lerner, Hans-Wolfram; Wagner, Matthias; Organometallics 27 (2008) 764–; doi:10.1021/om700995q

data_4070758
_publ_section_title
;
 Synthesis and Structural Characterization of the Diborylated
 Organometallics
 1,3-Bis(dibromoboryl)-1&#x2032;,2&#x2032;,3&#x2032;,4&#x2032;,5&#x2032;-(pentamethyl)ferrocene
 and 1,3-Bis(dibromoboryl)cymantrene
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              764
_journal_paper_doi               10.1021/om700995q
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C15 H18 B2 Br4 Fe'
_chemical_formula_weight         595.40
_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                 93.375(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.0877(10)
_cell_length_b                   18.6584(11)
_cell_length_c                   13.8304(11)
_cell_measurement_reflns_used    47387
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.7
_cell_measurement_theta_min      3.5
_cell_volume                     3886.7(5)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997) '
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990) '
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_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  0.0999
_diffrn_reflns_av_sigmaI/netI    0.0795
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            64011
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.80
_diffrn_reflns_theta_min         3.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.992
_exptl_absorpt_correction_T_max  0.2215
_exptl_absorpt_correction_T_min  0.1802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS (Spek, 2003; Blessing, 1995)'
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    2.035
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.718
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7368
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0709
_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^)+(0.0636P)^2^+12.9740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1701
_reflns_number_gt                5510
_reflns_number_total             7368
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om700995q-file001.cif
_cod_data_source_block           wa732
_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_sg_symbol_H-M      'P 21/c'
_cod_database_code               4070758