The molecular design of cage metal complexes for biological applications: pathways of the synthesis, and X-ray structures of a series of new N2-, S2- and O2-alicyclic iron(ii) di- and tetrachloroclathrochelates
Zelinskii, Genrikh E.; Belov, Alexander S.; Belaya, Irina G.; Vologzhanina, Anna V.; Novikov, Valentin V.; Varzatskii, Oleg A.; Voloshin, Yan Z.; New Journal of Chemistry 42 (2018) 56–; doi:10.1039/C7NJ03051G

data_7056755
_publ_section_title
;
 The molecular design of cage metal complexes for biological applications:
 pathways of the synthesis, and X-ray structures of a series of new N2-,
 S2- and O2-alicyclic iron(ii) di- and tetrachloroclathrochelates
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              56
_journal_paper_doi               10.1039/C7NJ03051G
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C16 H23 B2 Cl4 Fe N8 O6'
_chemical_formula_sum            'C16 H23 B2 Cl4 Fe N8 O6'
_chemical_formula_weight         642.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-10-27 deposited with the CCDC.
2017-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.700(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.453(2)
_cell_length_b                   12.533(3)
_cell_length_c                   23.913(5)
_cell_measurement_reflns_used    6300
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.81
_cell_measurement_theta_min      2.32
_cell_volume                     2552.8(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  apex
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_unetI/netI     0.0930
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            32919
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.656
_diffrn_reflns_theta_min         1.880
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.060
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       block
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.013
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         7798
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1480
_refine_ls_R_factor_gt           0.1140
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+60.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2425
_refine_ls_wR_factor_ref         0.2549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5315
_reflns_number_total             7798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj03051g2.cif
_cod_data_source_block           gz38
_cod_depositor_comments
'Adding full bibliography for 7056755--7056757.cif.'
_cod_original_cell_volume        2552.9(10)
_cod_database_code               7056755
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C14-C13 = C14A-C13 = C15A-C14A = C15-C14 = C16-C15A = C16-C15
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C14 \\sim C14A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C15A \\sim C15: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C15A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
4. Others
 Fixed Sof: H13A(0.5) H13B(0.5) C14(0.5) H14A(0.5) H14B(0.5) C15(0.5)
 H15A(0.5) H15B(0.5) H16A(0.5) H16B(0.5) H16C(0.5) H16D(0.5) H16E(0.5)
 H16F(0.5) C14A(0.5) H14C(0.5) H14D(0.5) C15A(0.5) H15C(0.5) H15D(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C14A(H14C,H14D), C15A(H15C,
 H15D)
5.b Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C16(H16D,H16E,H16F)
5.c Aromatic/amide H refined with riding coordinates:
 N7(H7), N8(H8)
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              30813