Series of High Spin Mononuclear Iron(III) Complexes with Schiff Base ligands derived from 2-hydroxybenzophenones
Pogány, Lukáš; Moncol, Jan; Pavlik, Jan; Salitros, Ivan; New J. Chem. 41 (2017) 5904–5915; doi:10.1039/C7NJ00617A

data_7056217
_publ_section_title
;
 Series of High Spin Mononuclear Iron(III) Complexes with Schiff Base
 ligands derived from 2-hydroxybenzophenones
;
_journal_issue                   13
_journal_name_full               'New J. Chem.'
_journal_page_first              5904
_journal_page_last               5915
_journal_paper_doi               10.1039/C7NJ00617A
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C33 H31 Br2 Fe N6 O2'
_chemical_formula_sum            'C33 H31 Br2 Fe N6 O2'
_chemical_formula_weight         759.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-01-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-01-05 deposited with the CCDC.
2017-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                101.157(2)
_cell_angle_beta                 96.653(2)
_cell_angle_gamma                110.337(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1152(3)
_cell_length_b                   13.0131(3)
_cell_length_c                   13.8985(4)
_cell_measurement_reflns_used    48268
_cell_measurement_temperature    110
_cell_measurement_theta_max      72.11
_cell_measurement_theta_min      3.31
_cell_volume                     1649.33(8)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      110.0
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36401
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         71.49
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'Genix3D Cu HF'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.819
_exptl_absorpt_correction_T_max  0.281
_exptl_absorpt_correction_T_min  0.194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   X-AREA
_exptl_crystal_colour            'reddish black'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       prism
_exptl_crystal_F_000             766
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6192
_refine_ls_number_restraints     486
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0568P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5224
_reflns_number_total             6192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00617a2.cif
_cod_data_source_block           lp239-2
_cod_database_code               7056217
_shelx_estimated_absorpt_t_max   0.579
_shelx_estimated_absorpt_t_min   0.270
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C19A) = Uanis(C19B)
Uanis(C18A) = Uanis(C18A)
Uanis(C17A) = Uanis(C17B)
Uanis(C35A) = Uanis(C35B)
Uanis(C16A) = Uanis(C16B)
Uanis(C15A) = Uanis(C15B)
Uanis(C14A) = Uanis(C14B)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{C14B, C15B, C16B, C17B, C14, C19B, C35B} sigma for 1-2: 0.01, 1-3: 0.04
as
{C14A, C15A, C16A, C17A, C18A, C19A, C35A}
5. Others
 Sof(C14B)=Sof(H14C)=Sof(H14D)=Sof(C15B)=Sof(H15C)=Sof(H15D)=Sof(C16B)=
 Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C14)=Sof(H14E)=Sof(H14F)=
 Sof(C19B)=Sof(H19C)=Sof(H19D)=Sof(C35B)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(1)
 Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(C16A)=
 Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(C18A)=Sof(H18A)=
 Sof(H18B)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(C35A)=Sof(H35A)=Sof(H35B)=
 Sof(H35C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C14A(H14A,H14B), C15A(H15A,H15B), C16A(H16A,H16B), C17A(H17A,H17B), C18A(H18A,
 H18B), C19A(H19A,H19B), C14B(H14C,H14D), C15B(H15C,H15D), C16B(H16C,H16D),
 C17B(H17C,H17D), C14(H14E,H14F), C19B(H19C,H19D)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C30(H30), C31(H31)
6.c Idealised Me refined as rotating group:
 C35A(H35A,H35B,H35C), C35B(H35D,H35E,H35F)
;
_shelx_fab_checksum              2942
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'