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_4350666
_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 Fe7.41 N54 O12, 4(Cl O4)'
_chemical_formula_sum            'C114 H84 Cl10 Fe7.41 N54 O28'
_chemical_formula_weight         3426.56
_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
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.309(11)
_cell_length_b                   20.309(11)
_cell_length_c                   22.404(6)
_cell_measurement_reflns_used    5659
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      3.0
_cell_volume                     9241(7)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      193(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
scan:
	Number of images: 302
	           Slice: -70.0000 - 81.0000
	     Image width: 0.5000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 50.0000
	          2theta: 20.0000
scan:
	Number of images: 346
	           Slice: -70.0000 - 103.0000
	     Image width: 0.5000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 50.0000
	          2theta: 20.0000
scan:
	Number of images: 296
	           Slice: -70.0000 - 78.0000
	     Image width: 0.5000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 0.0000
	             Phi: 0.0000
	             XTD: 50.0000
	          2theta: 20.0000
;
_diffrn_measurement_device
;
AFC8: Eulerian 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn70 (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.038880
_diffrn_orient_matrix_UB_12      -0.019174
_diffrn_orient_matrix_UB_13      0.021167
_diffrn_orient_matrix_UB_21      0.027254
_diffrn_orient_matrix_UB_22      0.038684
_diffrn_orient_matrix_UB_23      -0.012341
_diffrn_orient_matrix_UB_31      -0.013044
_diffrn_orient_matrix_UB_32      0.023675
_diffrn_orient_matrix_UB_33      0.037307
_diffrn_radiation_monochromator  'Graphite Monochromator with SHINE Optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1019
_diffrn_reflns_av_unetI/netI     0.1204
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28775
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.979
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3465
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
The PLATON SQUEEZE procedure was applied to recover 720 electrons per 
unit cell in one void (total volume 3111 ^A^3) that is 360 electrons 
per formula unit. The application of a solvent mask gave a significant 
improvement in the data statistics, however, this report is only intended 
to support the gross connectivity in the core of the structure.  Charge
balance has not been achieved and there is some question about the identity
of the atom at the site identified as Fe2, which refined to an occupancy of
0.602(4).
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13.
;
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         8074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0814
_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^)+(0.1563P)^2^+1.2070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2318
_refine_ls_wR_factor_ref         0.2598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5259
_reflns_number_total             8074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500348k_si_002.cif
_cod_data_source_block           Complex_4c
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' 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        9241(10)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4350666
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2.a Rotating group:
 N2(H2A,H2B)
2.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)
2.c X=CH2 refined with riding coordinates:
 N8(H8A,H8B), N11(H11A,H11B)
;
_shelx_estimated_absorpt_t_max   0.860
_shelx_estimated_absorpt_t_min   0.860
_shelx_fab_checksum              82036