Borylene-Based Functionalization of Iron-Alkynyl-σ-Complexes and Stepwise Reversible Metal-Boryl-to-Borirene Transformation: Synthesis, Characterization, and Density Functional Theory Studies
Holger Braunschweig; Qing Ye; Krzysztof Radacki; Peter Brenner; Gernot Frenking; Susmita De; Inorganic Chemistry 50 (2011) 62–71; doi:10.1021/ic1010874

data_4324082
_publ_contact_author_address
; Institut fuer Anorganische Chemie
Universitaet Wuerzburg
Am Hubland
97074 Wuerzburg, Germany
;
_publ_contact_author_email       H.Braunschweig@mail.uni-wuerzburg.de
_publ_contact_author_fax         +49-931-8884623
_publ_contact_author_name        'Prof. Dr. Holger Braunschweig'
_publ_contact_author_phone       +49-931-8885260
_publ_section_title
;
 Borylene-Based Functionalization of Iron-Alkynyl-\s-Complexes and
 Stepwise Reversible Metal-Boryl-to-Borirene Transformation: Synthesis,
 Characterization, and Density Functional Theory Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              62
_journal_page_last               71
_journal_paper_doi               10.1021/ic1010874
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C25 H38 B Fe N O Si2'
_chemical_formula_sum            'C25 H38 B Fe N O Si2'
_chemical_formula_weight         491.40
_chemical_name_common
;
?
;
_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                71.520(5)
_cell_angle_beta                 83.681(5)
_cell_angle_gamma                85.313(5)
_cell_formula_units_Z            4
_cell_length_a                   7.2055(8)
_cell_length_b                   19.729(2)
_cell_length_c                   19.868(2)
_cell_measurement_reflns_used    9344
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.65
_cell_measurement_theta_min      2.18
_cell_volume                     2659.2(5)
_computing_cell_refinement       'Saint+ ver. 7.53A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2008.3 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.53A (Bruker AXS)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            118503
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.79
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2008/1 (Brucker 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         11191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0418P)^2^+1.4860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0826
_reflns_number_gt                10113
_reflns_number_total             11191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1010874_si_002_2.cif
_cod_data_source_block           5
_cod_database_code               4324082