Synthesis and Characterization of a Terminal Borylene (Boranediyl) Complex
Alan H. Cowley; Viviana Lomelí; Andreas Voigt; Journal of the American Chemical Society 120 (1998) 6401–6402; doi:10.1021/ja9806433

data_4116743
_publ_section_title
;
 Synthesis and Characterization of a Terminal Borylene (Boranediyl)
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6401
_journal_page_last               6402
_journal_paper_doi               10.1021/ja9806433
_journal_volume                  120
_journal_year                    1998
_chemical_compound_source        selfmade
_chemical_formula_analytical     '[Fe(CO)4BC5(CH3)5]'
_chemical_formula_structural     '[Fe(CO)4BCp*]'
_chemical_formula_sum            'C14 H15 B Fe O4'
_chemical_formula_weight         313.92
_chemical_name_common            borylene-fe
_chemical_name_systematic
; 
 ? 
;
_chemical_temperature_decomposition 429
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.095(4)
_cell_length_b                   9.663(2)
_cell_length_c                   11.2943(14)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    178(2)
_cell_measurement_theta_max      28.483
_cell_measurement_theta_min      15.006
_cell_volume                     1429.1(6)
_computing_cell_refinement       'XSCANS version 2.10b (Siemens 1994)'
_computing_data_collection       'XSCANS version 2.10b (Siemens 1994)'
_computing_data_reduction        'XSCANS version 2.10b (Siemens 1994)'
_computing_molecular_graphics    'SHELXTL Plus version 5.03 (Siemens 1994)'
_computing_publication_material  'SHELXTL Plus version 5.03 (Siemens 1994)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      178(2)
_diffrn_measurement_device       Siemens-P4
_diffrn_measurement_method       'Theta / 2 Theta'
_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  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            2813
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.063
_exptl_absorpt_correction_T_max  n/a
_exptl_absorpt_correction_T_min  n/a
_exptl_absorpt_correction_type   n/a
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    n/a
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.767
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       n/a
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.001
_refine_ls_goodness_of_fit_obs   1.056
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1903
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.009
_refine_ls_restrained_S_obs      1.056
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_obs          0.0465
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1244
_refine_ls_wR_factor_obs         0.1170
_reflns_number_observed          1555
_reflns_number_total             1904
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9806433.cif
_cod_data_source_block           av58
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' 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^)+(0.0876P)^2^+0.0000P] 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^)+(0.0876P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1429.2(6)
_cod_database_code               4116743