Synthesis and structure of the first clathrochelate iron(II) tris-dioximates with inherent nitrile substituent(s) and new dehalogenation–reduction reaction at a quasi-aromatic macrobicyclic framework.
Voloshin, Yan Z.; Belov, Alexander S.; Varzatskii, Oleg A.; Shul'ga, Sergey V.; Stuzhin, Pavel A.; Starikova, Zoya A.; Lebed, Ekaterina G.; Bubnov, Yurii N.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 921–928; doi:10.1039/c1dt11285f

data_7017633
_publ_section_title
;
 Synthesis and structure of the first clathrochelate iron(II)
 tris-dioximates with inherent nitrile substituent(s) and new
 dehalogenation--reduction reaction at a quasi-aromatic macrobicyclic
 framework.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              921
_journal_page_last               928
_journal_paper_doi               10.1039/c1dt11285f
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C30 H20 B2 F2 Fe I2 N6 O6, 2(C6 H6)'
_chemical_formula_sum            'C42 H32 B2 F2 Fe I2 N6 O6'
_chemical_formula_weight         1086.01
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.307(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.266(4)
_cell_length_b                   10.531(3)
_cell_length_c                   27.206(7)
_cell_measurement_reflns_used    494
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     4373(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27556
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    1.819
_exptl_absorpt_correction_T_max  0.579
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998a)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.958
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0780
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0091P)^2^+135.0691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1577
_reflns_number_gt                4549
_reflns_number_total             5741
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1dt11285f.txt
_cod_data_source_block           fi
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4372.5(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7017633