Varied spin crossover behaviour in a family of dinuclear Fe(ii) triple helicate complexes.
Archer, Rosanna J.; Scott, Hayley S.; Polson, Matthew I. J.; Williamson, Bryce E.; Mathonière, Corine; Rouzières, Mathieu; Clérac, Rodolphe; Kruger, Paul E.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 7965–7974; doi:10.1039/c8dt01567h

data_7046459
_publ_section_title
;
 Varied spin crossover behaviour in a family of dinuclear Fe(ii) triple
 helicate complexes.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7965
_journal_page_last               7974
_journal_paper_doi               10.1039/c8dt01567h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C72 H66 Fe2 N24, 4(B F4), C H3 N0.5, C2 H3 N'
_chemical_formula_sum            'C75 H72 B4 F16 Fe2 N25.5'
_chemical_formula_weight         1789.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-04-09 deposited with the CCDC.
2018-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3905(4)
_cell_length_b                   22.6878(9)
_cell_length_c                   19.0917(6)
_cell_measurement_reflns_used    8769
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      73.7820
_cell_measurement_theta_min      3.0229
_cell_volume                     7965.8(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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      120(2)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
  1 omega  -84.00   33.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0313   19.0000  -90.0000 117

  2 omega  -49.00    6.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0313   37.0000    0.0000 55

  3 omega   26.00   77.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0313 -125.0000  120.0000 51

  4 omega   23.00   63.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0313 -125.0000    0.0000 40

  5 omega   36.00   99.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000    0.0000 63

  6 omega   33.00   72.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000  120.0000 39

  7 omega   39.00   94.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000 -180.0000 55

  8 omega  134.00  178.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  125.0000 -120.0000 44

  9 omega   30.00   87.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000   60.0000 57

 10 omega   41.00   67.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000 -150.0000 26

 11 omega   72.00   98.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000  120.0000 26

 12 omega   54.00   83.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000  -60.0000 29

 13 omega   18.00  135.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801    0.0000  -30.0000 117

 14 omega -119.00  -46.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0313  -77.0000 -150.0000 73
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33396
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.957
_diffrn_reflns_theta_min         3.093
_exptl_absorpt_coefficient_mu    3.783
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       needle
_exptl_crystal_F_000             3666
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         7964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.0879
_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^)+(0.1871P)^2^+9.0683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2606
_refine_ls_wR_factor_ref         0.3020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5046
_reflns_number_total             7964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01567h2.cif
_cod_data_source_block           rja72
_cod_depositor_comments
'Adding full bibliography for 7046459--7046462.cif.'
_cod_original_formula_sum        'C75 H72 B4 F16 Fe2 N25.50'
_cod_database_code               7046459
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C39(0.25) N14(0.25) C40(0.25) H40A(0.5) H40B(0.5) H40C(0.5)
 C37(0.5) N13(0.5) C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 N7(H7), N10(H10), N2(H2), C20(H20), C17(H17), C16(H16), C8(H8), C18(H18),
 C4(H4), C34(H34), C10(H10A), C7(H7A), C25(H25), C21(H21), C6(H6), C28(H28),
 C24(H24), C32(H32), C23(H23), C30(H30), C31(H31), C26(H26), C1(H1), C2(H2A)
3.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C36(H36A,H36B,H36C), C12(H12A,H12B,H12C), C40(H40A,H40B,
 H40C), C38(H38A,H38B,H38C)
;
_olex2_submission_special_instructions 'No special instructions were received'