Late First-Row Transition Metal Complexes of a Tetradentate Pyridinophane Ligand: Electronic Properties and Reactivity Implications
Julia R. Khusnutdinova; Jia Luo; Nigam P. Rath; Liviu M. Mirica; Inorganic Chemistry 52 (2013) 3920–3932; doi:10.1021/ic400260z

data_4334401
_publ_section_title
;
 Late First-Row Transition Metal Complexes of a Tetradentate Pyridinophane
 Ligand: Electronic Properties and Reactivity Implications
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3920
_journal_page_last               3932
_journal_paper_doi               10.1021/ic400260z
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C24 H32 F6 Fe N4 O6 S2'
_chemical_formula_sum            'C24 H32 F6 Fe N4 O6 S2'
_chemical_formula_weight         706.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2012-10-30
_audit_creation_method
;
  Olex2 1.2
  (compiled Oct 26 2012 17:09:49, GUI svn.r4371)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.203(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7740(12)
_cell_length_b                   16.483(2)
_cell_length_c                   18.281(2)
_cell_measurement_reflns_used    1371
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      17.22
_cell_measurement_theta_min      2.47
_cell_volume                     2889.0(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H.
 Puschmann,
OLEX2: a complete structure solution, refinement and analysis
 program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H.
 Puschmann,
OLEX2: a complete structure solution, refinement and analysis
 program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      153.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1801
_diffrn_reflns_av_unetI/netI     0.1028
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27565
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.990
_diffrn_reflns_theta_min         2.271
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0983 before and 0.0720 after correction.
The Ratio of minimum to maximum transmission is 0.7524.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.581
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         2547
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1587
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+17.0617P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.2160
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1397
_reflns_number_total             2547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic400260z_si_002_12.cif
_cod_data_source_block           m17611
_cod_depositor_comments
;Adding Fobs data.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'no' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4334401
_cod_database_fobs_code          4334401
_olex2_refinement_description
;1. Fixed Uiso At 1.2 times of: H4' of C4', {H6'1,H6'2} of C6', {H7'1,H7'2} of
 C7', H2 of C2, H3 of C3, H4 of C4, {H6A,H6B} of C6, {H7A,H7B} of C7 At 1.5
 times of: {H9A,H9B,H9C} of C9, {H9'1,H9'2,H9'3} of C9', {H10A,H10B,H10C} of
 C10, {H11A,H11B,H11C} of C11
2. Restrained distances C5'-C4' ~ C5-C4 ~ C4'-C3
 ~ C4-C3 ~ C3-C2 ~ C2-C1 with sigma of 0.01 N1-C1 ~ N1-C5' with sigma of 0.01
 C6'-C5' ~ C6-C5 with sigma of 0.01 N2-C6' ~ N2-C6 with sigma of 0.01 N2-C8' ~
 N2-C8 with sigma of 0.01 C8-C11 ~ C8'-C11 with sigma of 0.01 C8'-C10 ~ C8-C10
 with sigma of 0.01 S1-O1 ~ S1'-O1 with sigma of 0.01 S1-O3 ~ S1-O2 ~ S1'-O2'
 ~ S1'-O3' with sigma of 0.01 S1-C12 ~ S1'-C12' with sigma of 0.01 F2-C12 ~
 F2'-C12' ~ F1-C12 ~ F1'-C12' ~ F3'-C12' ~ F3-C12 with sigma of 0.01
3. Rigid
 bond restraints All non-hydrogen atoms with sigma for 1-2 distances of 0.01
 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and
 constraints
Uanis(O1) ~ Ueq, Uanis(O2) ~ Ueq, Uanis(O3) ~ Ueq, Uanis(O2') ~
 Ueq, Uanis(O3') ~ Ueq, Uanis(F1) ~ Ueq, Uanis(F2) ~ Ueq, Uanis(F3) ~ Ueq,
 Uanis(F1') ~ Ueq, Uanis(F2') ~ Ueq, Uanis(F3') ~ Ueq: with sigma of 0.1 and
 sigma for terminal atoms of 0.2
Uanis(F3) ~ Ueq, Uanis(F1') ~ Ueq, Uanis(F3')
 ~ Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C4) =
 Uanis(C4')
Uanis(C10) = Uanis(C11)
5. others
 Sof(S1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(O2)=Sof(O3)=Sof(C12)=1-Sof(F1)=1-Sof(F1)=
 1-Sof(F1)=1-Sof(F1)=1-Sof(F1)=1-Sof(F1)=1-Sof(F1)
 Sof(C4)=Sof(H4)=Sof(C5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=
 Sof(C8)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=1-Sof(H4)=1-Sof(H4)=1-Sof(H4)=1-
 Sof(H4)=1-Sof(H4)=1-Sof(H4)=1-Sof(H4)=1-Sof(H4)=1-Sof(H4)=1-Sof(H4)=1-Sof(H4)=
 1-Sof(H4)=1-Sof(H4)=1-Sof(H4)
6.a Secondary CH2 refined with riding
 coordinates: C6(H6A,H6B), C7(H7A,H7B), C6'(H6'1,H6'2), C7'(H7'1,H7'2)
6.b
 Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4),
 C4'(H4')
6.c Idealised Me refined as rotating group: C9(H9A,H9B,H9C),
 C9'(H9'1,H9'2,H9'3), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.669
_shelxl_version_number           2012-6