Direct monitoring of spin transitions in a dinuclear triple-stranded helicate iron(ii) complex through X-ray photoelectron spectroscopy.
Li, Li; Craze, Alexander R.; Akiyoshi, Ryohei; Tsukiashi, Asami; Hayami, Shinya; Mustonen, Outi; Bhadbhade, Mohan M.; Bhattacharyya, Saroj; Marjo, Christopher E.; Wang, Yun; Lindoy, Leonard F.; Aldrich-Wright, Janice R; Li, Feng; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2543–2548; doi:10.1039/c7dt04190j

data_7045260
_publ_section_title
;
 Direct monitoring of spin transitions in a dinuclear triple-stranded
 helicate iron(ii) complex through X-ray photoelectron spectroscopy.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2543
_journal_page_last               2548
_journal_paper_doi               10.1039/c7dt04190j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C60 H42 Fe2 N12 O3 S6, 2(C2 H3 N), 4(B F4), 0.25(O)'
_chemical_formula_sum            'C64 H48.6 B4 F16 Fe2 N14 O3.25 S6'
_chemical_formula_weight         1717.07
_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     dual
_audit_creation_date             2017-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2017-10-24 deposited with the CCDC.
2018-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                89.52(3)
_cell_angle_beta                 85.48(3)
_cell_angle_gamma                73.49(3)
_cell_formula_units_Z            2
_cell_length_a                   11.806(2)
_cell_length_b                   15.605(3)
_cell_length_c                   22.029(4)
_cell_measurement_reflns_used    2577
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2.26
_cell_volume                     3878.6(14)
_computing_cell_refinement       'ShelXL least squares'
_computing_data_collection       Blueice
_computing_data_reduction        XDS
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.907
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            47455
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.361
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       needle
_exptl_crystal_F_000             1737
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1153
_refine_ls_number_reflns         12382
_refine_ls_number_restraints     399
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1502P)^2^+5.4685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2157
_refine_ls_wR_factor_ref         0.2289
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10256
_reflns_number_total             12382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04190j2.cif
_cod_data_source_block           fl199-298k_a
_cod_depositor_comments
'Adding full bibliography for 7045259--7045260.cif.'
_cod_original_cell_volume        3878.6(15)
_cod_original_formula_sum        'C64 H48.60 B4 F16 Fe2 N14 O3.25 S6'
_cod_database_code               7045260
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F7AA-F8AA \\sim F7AA-F01Q \\sim F8AA-F02K \\sim F8AA-F01Q \\sim F02K-F01Q
 with sigma of 0.04
 F1-F3 \\sim F1-F4 \\sim F2-F3 \\sim F2-F4
 with sigma of 0.04
 B3-F1 \\sim B3-F2 \\sim B3-F3 \\sim B3-F4
 with sigma of 0.02
 F6AA-F9AA \\sim F6AA-F0BA \\sim F6AA-F00M \\sim F9AA-F0BA \\sim F0BA-F00M
 with sigma of 0.04
 B02Z-F6AA \\sim B02Z-F9AA \\sim B02Z-F0BA \\sim B02Z-F00M
 with sigma of 0.02
 F00N-F00W \\sim F00N-F5BA \\sim F00N-F9BA \\sim F00W-F5BA \\sim F00W-F9BA
\\sim F5BA-F9BA
 with sigma of 0.04
 B02P-F00N \\sim B02P-F00W \\sim B02P-F5BA \\sim B02P-F9BA
 with sigma of 0.02
 F0AA-F5 \\sim F0AA-F7 \\sim F0AA-F8
 with sigma of 0.04
 F6AA-F9AA \\sim F6AA-F0BA \\sim F6AA-F00M \\sim F7AA-F8AA \\sim F7AA-F01Q
\\sim F8AA-F02K \\sim F9AA-
 F0BA \\sim F0BA-F00M \\sim F02K-F01Q
 with sigma of 0.04
 B02Z-F6AA \\sim B02Z-F7AA \\sim B02Z-F8AA \\sim B02Z-F9AA \\sim B02Z-F0BA
\\sim B02Z-F02K \\sim B02Z-
 F00M \\sim B02Z-F01Q
 with sigma of 0.02
 F1-F3 \\sim F1-F4 \\sim F2-F3 \\sim F2-F4 \\sim F0AA-F5 \\sim F0AA-F7 \\sim
F0AA-F8 \\sim F5-F8
 with sigma of 0.04
 B3-F1 \\sim B3-F2 \\sim B3-F3 \\sim B3-F4 \\sim B3-F0AA \\sim B3-F5 \\sim
B3-F7 \\sim B3-F8
 with sigma of 0.02
 C1AB-C0AA \\sim C2-C1AA
 with sigma of 0.02
 N5AA-C1AB \\sim N3-C1AA
 with sigma of 0.02
 F2AA-F1AA \\sim F2AA-F4AA \\sim F2AA-F3AA \\sim F1AA-F3AA \\sim F4AA-F3AA
\\sim F2BA-F5AA \\sim F2BA-
 F3AB \\sim F5AA-F3AB \\sim F1BA-F3AB
 with sigma of 0.04
 B0AA-F2AA \\sim B0AA-F1AA \\sim B0AA-F4AA \\sim B0AA-F3AA \\sim B0AA-F2BA
\\sim B0AA-F5AA \\sim B0AA-
 F1BA \\sim B0AA-F3AB
 with sigma of 0.02
3. Rigid bond restraints
 F4AA, F5AA, F2BA, F1AA, F3AA, F3AB, F2AA, F1BA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Rigid body (RIGU) restrains
 F00M, F01Q, F7AA, F9AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F02K, F6AA, F8AA, F0BA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1AA, N3, N5AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F6AA, F7AA, F8AA, F9AA, F0BA, F02K, F00M, F01Q, B02Z
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B3, F1, F2, F3, F4, F0AA, F5, F7, F8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, N5AA, N3, C1AA, C1AB, C0AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B0AA, F2AA, F1AA, F4AA, F3AA, F2BA, F5AA, F1BA, F3AB
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Fe02, N4B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: C2(0.25) H2D(0.25) H2E(0.25) H2F(0.25) N5AA(0.25) N3(0.25)
 C1AA(0.25) N02V(0.5) C033(0.5) H03A(0.5) H03B(0.5) H03C(0.5) C02W(0.5)
 N0AA(0.25) C1(0.25) C4AA(0.25) H4AA(0.25) H4AB(0.25) H4AC(0.25) F6AA(0.5)
 F7AA(0.5) F8AA(0.5) F9AA(0.5) F0BA(0.5) F02K(0.5) F00M(0.5) F01Q(0.5) N1(0.5)
 C2AA(0.5) C3AA(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) F1(0.5) F2(0.5) F3(0.5)
 F4(0.5) F0AA(0.5) F5(0.5) F7(0.5) F8(0.5) O1(0.25) C1AB(0.25) C0AA(0.25)
 H0AA(0.25) H0AB(0.25) H0AC(0.25) N0AB(0.25) C5AA(0.25) C4AB(0.25) H4AD(0.25)
 H4AE(0.25) H4AF(0.25) F2AA(0.5) F1AA(0.5) F4AA(0.5) F3AA(0.5) F2BA(0.5)
 F5AA(0.5) F1BA(0.5) F3AB(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C4A(H4A), C6A(H6A), C7A(H7A), C9A(H9A), C10A(H10A),
 C12A(H12A), C13A(H13A), C15A(H15A), C16A(H16A), C17A(H17A), C19A(H19A),
 C20A(H20A), C1B(H1B), C2B(H2B), C4B(H4B), C5B(H5B), C6B(H6B), C8B(H8B),
 C9B(H9B), C11B(H11B), C12B(H12B), C14B(H14B), C15B(H15B), C16B(H16B),
 C18B(H18B), C19B(H19B), C1C(H1C), C2C(H2C), C4C(H4C), C5C(H5C), C6C(H6C),
 C8C(H8C), C9C(H9C), C11C(H11C), C12C(H12C), C14C(H14C), C15C(H15C), C16C(H16C),
  C18C(H18C), C19C(H19C)
6.b Idealised Me refined as rotating group:
 C2(H2D,H2E,H2F), C033(H03A,H03B,H03C), C4AA(H4AA,H4AB,H4AC), C3AA(H3AA,H3AB,
 H3AC), C0AA(H0AA,H0AB,H0AC), C4AB(H4AD,H4AE,H4AF)
;
_olex2_submission_special_instructions 'No special instructions were received'