Regulation of Iron-Catalyzed Olefin Hydroboration by Ligand Modifications at a Remote Site
Tseng, Kuei-Nin T.; Kampf, Jeff W.; Szymczak, Nathaniel K.; ACS Catalysis 5 (2015) 411–; doi:10.1021/cs501820w

data_4512491
_publ_section_title
;
 Regulation of Iron-Catalyzed Olefin Hydroboration by Ligand Modifications
 at a Remote Site
;
_journal_issue                   1
_journal_name_full               'ACS Catalysis'
_journal_page_first              411
_journal_paper_doi               10.1021/cs501820w
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C23 H19 F6 Fe N5 O6 S2'
_chemical_formula_sum            'C23 H19 F6 Fe N5 O6 S2'
_chemical_formula_weight         695.40
_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                66.351(5)
_cell_angle_beta                 73.133(5)
_cell_angle_gamma                69.747(5)
_cell_formula_units_Z            2
_cell_length_a                   10.7036(2)
_cell_length_b                   12.1278(2)
_cell_length_c                   12.2733(9)
_cell_measurement_reflns_used    25439
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.30
_cell_measurement_theta_min      4.00
_cell_volume                     1347.80(12)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r12'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r12'
_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      85(2)
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku Saturn944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'micro-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            38231
_diffrn_reflns_theta_full        68.23
_diffrn_reflns_theta_max         68.23
_diffrn_reflns_theta_min         3.99
_exptl_absorpt_coefficient_mu    6.781
_exptl_absorpt_correction_T_max  0.5504
_exptl_absorpt_correction_T_min  0.2929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0030(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         4866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0530P)^2^+1.3580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                4802
_reflns_number_total             4866
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs501820w_si_001.cif
_cod_data_source_block           kt2293
_cod_depositor_comments
'Adding full bibliography for 4512489--4512491.cif.'
_cod_original_cell_volume        1347.80(10)
_cod_database_code               4512491