Formation of iron(iii)‒thiolate metallocyclophane using a ferrocene-based bis-isocyanide
Huang, Yen-Chung; Lan, Wan-Yu; Ching, Wei-Min; Hsu, Sodio C. N.; New Journal of Chemistry 44 (2020) 18242–18249; doi:10.1039/D0NJ03967E

data_7060018
_publ_section_title
;
 Formation of iron(iii)--thiolate metallocyclophane using a
 ferrocene-based bis-isocyanide
;
_journal_issue                   42
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18242
_journal_page_last               18249
_journal_paper_doi               10.1039/D0NJ03967E
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         '1.25(C9.6 H8 Fe0.8 N1.6), 0.5(O2)'
_chemical_formula_sum            'C12 H8 Fe N2 O'
_chemical_formula_weight         252.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-05-18
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-09-06 deposited with the CCDC.	2020-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.19(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.076(5)
_cell_length_b                   8.347(4)
_cell_length_c                   13.309(9)
_cell_measurement_reflns_used    9064
_cell_measurement_temperature    199.99
_cell_measurement_theta_max      25.040
_cell_measurement_theta_min      2.296
_cell_volume                     957.9(10)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      199.99
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3616
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.038
_diffrn_reflns_theta_max         25.038
_diffrn_reflns_theta_min         3.222
_exptl_absorpt_coefficient_mu    1.547
_exptl_absorpt_correction_T_max  0.9543
_exptl_absorpt_correction_T_min  0.7038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       prism
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         843
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.196
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+11.2372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1978
_refine_ls_wR_factor_ref         0.2183
_reflns_Friedel_coverage         0.000
_reflns_number_gt                694
_reflns_number_total             843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03967e2.cif
_cod_data_source_block           FcNC2
_cod_depositor_comments
'Adding full bibliography for 7060017--7060019.cif.'
_cod_original_cell_volume        957.8(9)
_cod_database_code               7060018
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.886
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C5'-C1'
 1.4 with sigma of 0.02
 C1'-C2'
 1.45 with sigma of 0.02
 C2'-C3'
 1.4 with sigma of 0.02
 C3'-C4'
 1.45 with sigma of 0.02
 C5'-N1'
 1.4 with sigma of 0.02
 N1'-C6'
 1.16 with sigma of 0.02
 C5'-C4'
 1.42 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(N1')
Uanis(C6) = Uanis(C6')
Uanis(C1) = Uanis(C4)
Uanis(C3') = Uanis(C4') = Uanis(C5') = Uanis(C1') = Uanis(C2') = Uanis(C1)
4. Others
 Fixed Sof: C1(0.8) H1(0.8) C2(0.8) H2(0.8) C3(0.8) H3(0.8) C4(0.8) H4(0.8)
 C5(0.8) C6(0.8) H6(0.8) N1(0.8) C1'(0.2) H1'(0.2) C2'(0.2) H2'(0.2) C3'(0.2)
 H3'(0.2) C4'(0.2) H4'(0.2) C5'(0.2) C6'(0.2) H6'(0.2) N1'(0.2) Fe1(0.4)
 Fe2(0.1) O1(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C1'(H1'), C2'(H2'), C3'(H3'), C4'(H4')
5.b :
 C6(H6), C6'(H6')
;
_shelx_res_checksum              18358
_olex2_submission_special_instructions 'No special instructions were received'