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_7056757
_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
'1.5(C18 H26 B2 Cl2 Fe N6 O6 S4), 0.5(C20 H30 B2 Fe N6 O6 S6)'
_chemical_formula_sum            'C37 H54 B4 Cl3 Fe2 N12 O12 S9'
_chemical_formula_weight         1408.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-12-24
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_audit_update_record
;
2015-10-27 deposited with the CCDC.
2017-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                117.4170(10)
_cell_angle_beta                 99.084(2)
_cell_angle_gamma                107.0350(10)
_cell_formula_units_Z            2
_cell_length_a                   14.4860(4)
_cell_length_b                   15.3721(3)
_cell_length_c                   15.7873(4)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    120
_cell_measurement_theta_max      67.70
_cell_measurement_theta_min      3.34
_cell_volume                     2800.59(13)
_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., 2013)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35554
_diffrn_reflns_theta_full        67.77
_diffrn_reflns_theta_max         67.77
_diffrn_reflns_theta_min         3.34
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.191
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.876
_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    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1446
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         9471
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0100P)^2^+12.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                7854
_reflns_number_total             9471
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj03051g2.cif
_cod_data_source_block           gz59
_cod_depositor_comments
'Adding full bibliography for 7056755--7056757.cif.'
_cod_original_cell_volume        2800.58(12)
_cod_database_code               7056757
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S9-C37A
 1.7 with sigma of 0.02
 C38A-S10
 1.7 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C37A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C38A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uiso(Cl1) = Uiso(S9) = Uiso(S10) = Uiso(Cl2A)
4. Others
 Fixed Sof: Cl1(0.5) S10(0.5) S9(0.5) Cl2A(0.5) C37A(0.5) H37A(0.5) H37B(0.5)
 C38A(0.5) H38A(0.5) H38B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B), C5(H5A,H5B), C6(H6A,H6B), C9(H9A,H9B), C10(H10A,H10B),
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C37A(H37A,H37B), C38A(H38A,H38B)
5.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C36(H36A,H36B,H36C), C14(H14A,H14B,H14C), C18(H18A,H18B,
 H18C)
;
_shelx_res_checksum              8230