Electronic Perturbations of Iron Dipyrrinato Complexes via Ligand β-Halogenation and meso-Fluoroarylation
Austin B. Scharf; Theodore A. Betley; Inorganic Chemistry 50 (2011) 6837–6845; doi:10.1021/ic2009539

data_4325712
_publ_contact_author_address
;
Department of Chemistry and Chemical Biology 
Harvard University
12 Oxford St
Cambridge, MA 02138 (USA)
;
_publ_contact_author_email       contact-betley@chemistry.harvard.edu
_publ_contact_author_name        'Prof. Theodore Betley'
_publ_section_title
;
 Electronic Perturbations of Iron Dipyrrinato Complexes via Ligand
 \b-Halogenation and meso-Fluoroarylation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6837
_journal_page_last               6845
_journal_paper_doi               10.1021/ic2009539
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C40 H34 Cl F6 Fe N3'
_chemical_formula_weight         762.00
_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                96.774(2)
_cell_angle_beta                 100.237(2)
_cell_angle_gamma                93.746(2)
_cell_formula_units_Z            2
_cell_length_a                   8.0378(8)
_cell_length_b                   13.8834(13)
_cell_length_c                   16.5650(15)
_cell_measurement_reflns_used    29233
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      14.572
_cell_measurement_theta_min      2.326
_cell_volume                     1799.3(3)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker D8 goniometer with CCD area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'diamond 1 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29174
_diffrn_reflns_theta_full        14.59
_diffrn_reflns_theta_max         14.59
_diffrn_reflns_theta_min         0.86
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.9970
_exptl_absorpt_correction_T_min  0.9654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         6421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0425P)^2^+2.1034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1097
_reflns_number_gt                5122
_reflns_number_total             6421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2009539_si_002_1.cif
_cod_data_source_block           as1_0m
_cod_database_code               4325712