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_7056756
_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_absolute_configuration ad
_chemical_formula_moiety         'C32 H30 B2 Fe N6 O12'
_chemical_formula_sum            'C32 H30 B2 Fe N6 O12'
_chemical_formula_weight         768.09
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0772(2)
_cell_length_b                   11.0772(2)
_cell_length_c                   26.6909(9)
_cell_measurement_reflns_used    9759
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      2.39
_cell_volume                     3275.09(14)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            29809
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         1.99
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0568 before and 0.0506 after correction.
The Ratio of minimum to maximum transmission is 0.8566.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0500P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                4529
_reflns_number_total             4981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj03051g2.cif
_cod_data_source_block           gz94
_cod_depositor_comments
'Adding full bibliography for 7056755--7056757.cif.'
_cod_database_code               7056756
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.02) H4(0.025) H5(0.029) H6(0.026) H9A(0.017) H9B(0.017)
 H10A(0.022) H10B(0.022) H11A(0.025) H11B(0.025) H12A(0.037) H12B(0.037)
 H12C(0.037) H15(0.022) H16(0.025)
 Fixed X: H3(-0.6618) H4(-0.597) H5(-0.462) H6(-0.3879) H9A(-0.7098) H9B(-
 0.8267) H10A(-0.7783) H10B(-0.6558) H11A(-0.8913) H11B(-0.769) H12A(-0.8384)
 H12B(-0.8276) H12C(-0.7086) H15(0.0108) H16(0.0791)
 Fixed Y: H3(0.7788) H4(0.9658) H5(1.0843) H6(1.0163) H9A(0.247) H9B(0.2784)
 H10A(0.1242) H10B(0.0964) H11A(0.0449) H11B(0.0191) H12A(-0.0976) H12B(-
 0.1618) H12C(-0.1165) H15(0.23) H16(0.0402)
 Fixed Z: Fe1(0.25) H3(0.4584) H4(0.4902) H5(0.4447) H6(0.3671) H9A(0.382)
 H9B(0.3492) H10A(0.2918) H10B(0.321) H11A(0.3594) H11B(0.3896) H12A(0.2983)
 H12B(0.3518) H12C(0.3234) H15(0.1976) H16(0.2237)
;
_shelx_res_checksum              12915
_olex2_submission_special_instructions 'No special instructions were received'