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_7045259
_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, 4(C2 H3 N), 4(B F4), 0.5(H2 O)'
_chemical_formula_sum            'C68 H55 B4 F16 Fe2 N16 O3.5 S6'
_chemical_formula_weight         1803.58
_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   mixed
_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                89.79(3)
_cell_angle_beta                 85.72(3)
_cell_angle_gamma                73.09(3)
_cell_formula_units_Z            2
_cell_length_a                   11.724(2)
_cell_length_b                   15.555(3)
_cell_length_c                   21.641(4)
_cell_measurement_reflns_used    2568
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      2.26
_cell_volume                     3764.8(13)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.904
_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  0.0247
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.912
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54362
_diffrn_reflns_point_group_measured_fraction_full 0.912
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         1.368
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       prism
_exptl_crystal_F_000             1830
_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         0.634
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1115
_refine_ls_number_reflns         14128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0523P)^2^+4.3339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12552
_reflns_number_total             14128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04190j2.cif
_cod_data_source_block           fl199_a
_cod_depositor_comments
'Adding full bibliography for 7045259--7045260.cif.'
_cod_original_cell_volume        3764.8(14)
_cod_original_formula_sum        'C68 H55 B4 F16 Fe2 N16 O3.50 S6'
_cod_database_code               7045259
_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, All O(H,H) groups
2. Others
 Fixed Sof: F2(0.2) F3(0.3) F15(0.3) F2AA(0.2) F02H(0.7) F00K(0.7) F01T(0.8)
 F00X(0.8) F1(0.5) F011(0.6) F034(0.5) F035(0.5) F01A(0.5) F0AA(0.4) O1(0.5)
 H1G(0.5) H1H(0.5)
3.a Free rotating group:
 O1(H1G,H1H)
3.b 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), C6B(H6B), C7B(H7B), C9B(H9B),
 C10B(H10B), C12B(H12B), C13B(H13B), C15B(H15B), C16B(H16B), C17B(H17B),
 C19B(H19B), C20B(H20B), C1C(H1C), C2C(H2C), C4C(H4C), C6C(H6C), C7C(H7C),
 C9C(H9C), C10C(H10C), C12C(H12C), C13C(H13C), C15C(H15C), C16C(H16C),
 C17C(H17C), C19C(H19C), C20C(H20C)
3.c Idealised Me refined as rotating group:
 C1(H1D,H1E,H1F), C032(H03A,H03B,H03C), C02X(H02A,H02B,H02C), C02Y(H02D,H02E,
 H02F)
;
_olex2_submission_special_instructions 'No special instructions were received'