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_4512490
_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         'C25 H24 F3 Fe N5 O4 S'
_chemical_formula_sum            'C25 H24 F3 Fe N5 O4 S'
_chemical_formula_weight         603.40
_space_group_IT_number           1
_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                99.732(7)
_cell_angle_beta                 90.796(6)
_cell_angle_gamma                112.598(8)
_cell_formula_units_Z            2
_cell_length_a                   8.4756(2)
_cell_length_b                   8.8071(3)
_cell_length_c                   18.6806(13)
_cell_measurement_reflns_used    18072
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.20
_cell_measurement_theta_min      2.40
_cell_volume                     1264.06(13)
_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, TWINSOLVE'
_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 29.257
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0957
_diffrn_reflns_av_sigmaI/netI    0.1035
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34990
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    6.140
_exptl_absorpt_correction_T_max  0.8870
_exptl_absorpt_correction_T_min  0.6394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.268
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         8338
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1322P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2118
_refine_ls_wR_factor_ref         0.2194
_reflns_number_gt                7206
_reflns_number_total             8338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs501820w_si_001.cif
_cod_data_source_block           kt2300
_cod_depositor_comments
'Adding full bibliography for 4512489--4512491.cif.'
_cod_database_code               4512490