Oligonuclear Fe complexes (Fe, Fe4, Fe6, Fe9) derived from tritopic pyridine bis-hydrazone ligands-structural, magnetic, and Mössbauer studies.
Anwar, Muhammad U.; Dawe, Louise N.; Parsons, Stewart R.; Tandon, Santokh S.; Thompson, Laurence K.; Dey, Subrata K.; Mereacre, Valeriu; Reiff, William M.; Bunge, Scott D.; Inorganic chemistry 53 (2014) 4655–4668; doi:10.1021/ic500348k

data_4350664
_publ_section_title
;
 Oligonuclear Fe complexes (Fe, Fe4, Fe6, Fe9) derived from tritopic
 pyridine bis-hydrazone ligands-structural, magnetic, and M\"ossbauer
 studies.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4655
_journal_page_last               4668
_journal_paper_doi               10.1021/ic500348k
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety
'C114 H84 Cl6 Fe6.85 N54 O12, 8(Cl O4), 5(C H4 O), 4.5(C2 H3 N)'
_chemical_formula_sum            'C128 H117.5 Cl14 Fe6.86 N58.5 O49'
_chemical_formula_weight         4138.65
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-08-26
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.116(2)
_cell_length_b                   20.116(2)
_cell_length_c                   21.630(2)
_cell_measurement_reflns_used    35089
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.9874
_cell_measurement_theta_min      2.0247
_cell_volume                     8752.7(15)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_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  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2013)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            68990
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.025
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.862
_exptl_absorpt_correction_T_max  0.8024
_exptl_absorpt_correction_T_min  0.7064
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'T. Higashi, 2000'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4207
_exptl_crystal_size_max          0.445
_exptl_crystal_size_mid          0.392
_exptl_crystal_size_min          0.351
_refine_diff_density_max         1.704
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         7707
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0972
_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^)+(0.1771P)^2^+23.7770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2810
_refine_ls_wR_factor_ref         0.2834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7424
_reflns_number_total             7707
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500348k_si_002.cif
_cod_data_source_block           Complex_4a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Numerical' was
changed to 'numerical' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        8752(2)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_original_formula_sum        'C128 H117.50 Cl14 Fe6.86 N58.50 O49'
_cod_database_code               4350664
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H30A,H30B,H30C} of C30, All N(H,H) groups
 At 1.5 times of:
  {H31A,H31B,H31C} of C31
2. Uiso/Uaniso restraints and constraints
C24 \\sim C23 \\sim C22 \\sim C21 \\sim C20 \\sim N10: within 1.7A 
with sigma of 0.008 and sigma for terminal atoms of 0.016
Cl5 \\sim Cl4 \\sim O9 \\sim O8 \\sim O10 \\sim O11 \\sim O12 
\\sim O14: within 1.7A with sigma of 0.008 and sigma for terminal 
atoms of 0.016
O16 \\sim C35: within 1.7A with sigma of 0.004 and sigma for terminal 
atoms of 0.008
N15 \\sim C32 \\sim C31: within 1.7A with sigma of 0.004 and sigma for 
terminal atoms of 0.008
Uanis(O14) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms 
of 0.002
3. Others
 Sof(Cl5)=Sof(O12)=Sof(O14)=1-FVAR(1)
 Sof(Cl4)=Sof(O8)=Sof(O9)=FVAR(1)
 Fixed Sof: O16(0.25) C35(0.25) N15(0.75) N16(0.375) C31(0.75) H31A(0.75)
 H31B(0.75) H31C(0.75) C32(0.75) C33(0.375) C34(0.375)
4.a Me refined with riding coordinates:
 C30(H30A,H30B,H30C)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C11(H11), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C28(H28)
4.c X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N8(H8A,H8B), N11(H11A,H11B)
4.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C)
;
_shelx_estimated_absorpt_t_max   0.752
_shelx_estimated_absorpt_t_min   0.700
_shelxl_version_number           2013-4