Iron(iii) bis(pyrazol-1-yl)acetate based decanuclear metallacycles: synthesis, structure, magnetic properties and DFT calculations.
Gajewska, Małgorzata J; Bieńko, Alina; Herchel, Radovan; Haukka, Matti; Jerzykiewicz, Maria; Ożarowski, Andrzej; Drabent, Krzysztof; Hung, Chen-Hsiung; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15089–15096; doi:10.1039/c6dt02333a

data_7040293
_publ_section_title
;
 Iron(iii) bis(pyrazol-1-yl)acetate based decanuclear metallacycles:
 synthesis, structure, magnetic properties and DFT calculations.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15089
_journal_page_last               15096
_journal_paper_doi               10.1039/c6dt02333a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C260 H450 Fe10 N40 O40'
_chemical_formula_sum            'C260 H450 Fe10 N40 O40'
_chemical_formula_weight         5335.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-03-17 deposited with the CCDC.
2016-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.3510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.8248(3)
_cell_length_b                   24.7952(3)
_cell_length_c                   28.7437(3)
_cell_measurement_reflns_used    145680
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.8650
_cell_measurement_theta_min      1.6620
_cell_volume                     16979.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1717
_diffrn_reflns_av_unetI/netI     0.1114
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            466223
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.085
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.043
_exptl_crystal_description       prism
_exptl_crystal_F_000             5740
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
The contribution of the missing solvent to the calculated structure factors
was taken into account with the BYPASS algorithm (van der Sluis & Spek, 1990),
implemented as the SQUEEZE option in PLATON (Spek, 2003).
;
_refine_diff_density_max         3.454
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.374
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1525
_refine_ls_number_reflns         28380
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.805
_refine_ls_R_factor_all          0.1968
_refine_ls_R_factor_gt           0.1316
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3602
_refine_ls_wR_factor_ref         0.4034
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16294
_reflns_number_total             28380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02333a2.cif
_cod_data_source_block           i15626_7_sq
_cod_depositor_comments
;Adding full bibliography for 7040293.cif.

 Adding full bibliography for 7040293.cif.
;
_cod_database_code               7040293
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.903
_shelx_estimated_absorpt_t_max   0.954
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              38116
_shelx_fab_checksum              24937