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_7046462
_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), C0.5 H0.5 Cl2, O'
_chemical_formula_sum            'C72.5 H66.5 B4 Cl2 F16 Fe2 N24 O'
_chemical_formula_weight         1819.83
_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
_audit_creation_date             2017-03-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-03-08 deposited with the CCDC.
2018-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                73.358(4)
_cell_angle_beta                 76.332(5)
_cell_angle_gamma                73.466(5)
_cell_formula_units_Z            2
_cell_length_a                   14.1516(9)
_cell_length_b                   16.1395(8)
_cell_length_c                   24.9544(11)
_cell_measurement_reflns_used    8603
_cell_measurement_temperature    240.43(10)
_cell_measurement_theta_max      73.4050
_cell_measurement_theta_min      2.9340
_cell_volume                     5160.2(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      240.43(10)
_diffrn_detector_area_resol_mean 5.3250
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_details
;
  1 omega -105.00   -8.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9063  -77.0000 -150.0000 97

  2 omega  -42.00   17.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9063   37.0000  -30.0000 59

  3 omega  -96.00   -3.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9063  125.0000  -30.0000 93

  4 omega -111.00  -11.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9063  -57.0000   90.0000 100

  5 omega  -45.00   -4.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000   30.0000   30.0000 41

  6 omega -105.00  -80.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000  -94.0000   90.0000 25

  7 omega   24.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -94.0000   30.0000 85

  8 omega   32.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -94.0000 -150.0000 65

  9 omega   48.00   74.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -94.0000 -180.0000 26

 10 omega   27.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -94.0000  120.0000 82

 11 omega   79.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   30.0000  -90.0000 99

 12 omega   36.00   62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000  -30.0000 26

 13 omega   31.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000   90.0000 58

 14 omega   67.00  120.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801 -125.0000  -30.0000 53

 15 omega   94.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  125.0000   90.0000 80

 16 omega   30.00   84.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000    0.0000 54

 17 omega   68.00   94.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000    0.0000 26

 18 omega   63.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000 -150.0000 26

 19 omega   39.00   80.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000 -150.0000 41

 20 omega   93.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   45.0000    0.0000 83
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0733582000
_diffrn_orient_matrix_UB_12      -0.0195609000
_diffrn_orient_matrix_UB_13      -0.0537315000
_diffrn_orient_matrix_UB_21      0.0698400000
_diffrn_orient_matrix_UB_22      0.0498255000
_diffrn_orient_matrix_UB_23      0.0101035000
_diffrn_orient_matrix_UB_31      0.0548921000
_diffrn_orient_matrix_UB_32      -0.0873487000
_diffrn_orient_matrix_UB_33      0.0358319000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_av_unetI/netI     0.1337
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            37020
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.627
_diffrn_reflns_theta_min         2.939
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.396
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       block
_exptl_crystal_F_000             1855
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.906
_refine_diff_density_min         -1.858
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.241
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         20325
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.241
_refine_ls_R_factor_all          0.1987
_refine_ls_R_factor_gt           0.1484
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3795
_refine_ls_wR_factor_ref         0.4516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9740
_reflns_number_total             20325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01567h2.cif
_cod_data_source_block           rja92
_cod_depositor_comments
'Adding full bibliography for 7046459--7046462.cif.'
_cod_original_formula_sum        'C72.50 H66.50 B4 Cl2 F16 Fe2 N24 O'
_cod_database_code               7046462
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C72H66B4N24F16Fe2
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B4-F13 = B4-F14 = B4-F15 = B4-F16
 1.33 with sigma of 0.01
 F13-F14
 2.2 with sigma of 0.01
 F13-F15
 2.2 with sigma of 0.01
 F13-F16
 2.2 with sigma of 0.01
 F14-F15
 2.2 with sigma of 0.01
 F14-F16
 2.2 with sigma of 0.01
 F15-F16
 2.2 with sigma of 0.01
3. Others
 Fixed Sof: Cl3(0.5) Cl2(0.5) C73(0.5) H73(0.5)
 Fixed Uiso: F7(0.15) B2(0.15) F6(0.15) F5(0.15) F8(0.15) F15(0.15) B4(0.15)
 F16(0.15) F13(0.15) F14(0.15)
4.a Ternary CH refined with riding coordinates:
 C73(H73)
4.b Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C68(H68), C34(H34), N10(H10), N2(H2), C58(H58), N24(H24), C44(H44),
 C16(H16), C28(H28), C20(H20), N0AA(H0AA), C4(H4), C8(H8), C66(H66), C64(H64),
 C41(H41), C65(H65), C32(H32), C40(H40), C30(H30), C42(H42), C69(H69), C19(H19),
  C52(H52), C54(H54), C21(H21), C31(H31), N16(H16A), C55(H55), C56(H56),
 C18(H18), C9(H9), C10(H10A), C45(H45), C2(H2A), N8(H8A), C71(H71), C1(H1),
 C72(H72), C48(H48), C26(H26), C25(H25), C23(H23), C24(H24A), C47(H47)
4.d Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C12(H12A,H12B,H12C), C36(H36A,H36B,H36C), C60(H60A,H60B,
 H60C), C38(H38A,H38B,H38C), C14(H14A,H14B,H14C)
;
_olex2_submission_special_instructions 'No special instructions were received'