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_7046461
_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, C H Cl3, 4(B F4), C2 H3 N, 0.5(O)'
_chemical_formula_sum            'C75 H70 B4 Cl3 F16 Fe2 N25 O0.5'
_chemical_formula_weight         1894.85
_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                73.547(3)
_cell_angle_beta                 75.732(3)
_cell_angle_gamma                73.498(3)
_cell_formula_units_Z            2
_cell_length_a                   13.9106(5)
_cell_length_b                   15.9337(6)
_cell_length_c                   24.8612(9)
_cell_measurement_reflns_used    10825
_cell_measurement_temperature    279.17(10)
_cell_measurement_theta_max      73.8675
_cell_measurement_theta_min      2.9694
_cell_volume                     4983.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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      279.17(10)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -65.00   17.00   1.0000    2.2300
omega____ theta____ kappa____ phi______ frames
    -      -39.9063   57.0000  -90.0000 82

  2 omega -105.00   43.00   1.0000    2.2300
omega____ theta____ kappa____ phi______ frames
    -      -39.9063    0.0000 -120.0000 148

  3 omega   27.00   81.00   1.0000    2.2300
omega____ theta____ kappa____ phi______ frames
    -       39.9063 -125.0000 -180.0000 54

  4 omega   29.00   89.00   1.0000    2.2300
omega____ theta____ kappa____ phi______ frames
    -       39.9063 -125.0000   30.0000 60

  5 omega -125.00  -75.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      -61.5000 -125.0000  -60.0000 50

  6 omega   78.00  178.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      107.7801   30.0000  120.0000 100

  7 omega   38.00   91.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000   60.0000 53

  8 omega   50.00   76.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -61.0000  150.0000 26

  9 omega   62.00   90.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      107.7801 -125.0000  -30.0000 28

 10 omega   46.00  106.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -94.0000   90.0000 60

 11 omega   54.00   91.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000  -30.0000 37

 12 omega   31.00   84.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000  120.0000 53

 13 omega   35.00   64.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000  -30.0000 29

 14 omega   31.00   82.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000 -150.0000 51

 15 omega   30.00   60.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -77.0000  -60.0000 30

 16 omega   49.00   96.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -94.0000  150.0000 47

 17 omega   82.00  178.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      107.7801   30.0000   30.0000 96

 18 omega   90.00  116.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -61.0000  150.0000 26

 19 omega   96.00  128.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -77.0000  -60.0000 32

 20 omega   36.00  116.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      107.7801 -113.0000 -103.0000 80

 21 omega   42.00   69.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000   30.0000 27

 22 omega   30.00  112.00   1.0000    9.1600
omega____ theta____ kappa____ phi______ frames
    -      107.7801 -113.0000   12.0000 82
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0926564000
_diffrn_orient_matrix_UB_12      -0.0541019000
_diffrn_orient_matrix_UB_13      -0.0342577000
_diffrn_orient_matrix_UB_21      -0.0173608000
_diffrn_orient_matrix_UB_22      0.0730846000
_diffrn_orient_matrix_UB_23      -0.0547834000
_diffrn_orient_matrix_UB_31      0.0700305000
_diffrn_orient_matrix_UB_32      0.0496526000
_diffrn_orient_matrix_UB_33      0.0118573000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34551
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.999
_diffrn_reflns_theta_min         2.972
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.777
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       block
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.945
_refine_diff_density_min         -1.587
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1120
_refine_ls_number_reflns         17779
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0832
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1444P)^2^+6.1663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2333
_refine_ls_wR_factor_ref         0.2546
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13467
_reflns_number_total             17779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01567h2.cif
_cod_data_source_block           rja79
_cod_depositor_comments
'Adding full bibliography for 7046459--7046462.cif.'
_cod_original_formula_sum        'C75 H70 B4 Cl3 F16 Fe2 N25 O0.50'
_cod_database_code               7046461
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C72H66B4N24F16Fe2
_reflns_odcompleteness_completeness 99.95
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F14-B4
 1.3 with sigma of 0.02
 F13'-B4
 1.3 with sigma of 0.02
 F13-F15
 2.2 with sigma of 0.01
 F16-F13
 2.2 with sigma of 0.01
 F14-F15
 2.2 with sigma of 0.01
 F16-F15
 2.2 with sigma of 0.01
 F16-F14
 2.2 with sigma of 0.01
 F13-F14
 2.2 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(F14')=Sof(F15')=Sof(F16')=Sof(F13')=1-FVAR(1)
 Sof(F13)=Sof(F15)=Sof(F16)=Sof(F14)=FVAR(1)
 Fixed Sof: O1(0.5)
 Fixed Uiso: B4(0.1) F13(0.1) F15(0.1) F16(0.1) F14(0.1) F14'(0.1) F15'(0.1)
 F16'(0.1) F13'(0.1)
5.a Ternary CH refined with riding coordinates:
 C78(H78)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N18(H18), N10(H10), C6(H6), C58(H58), N24(H24), C10(H10A), N8(H8),
 C16(H16), C44(H44), C32(H32), C1(H1), C69(H69), C68(H68), C34(H34), C8(H8A),
 C20(H20), C4(H4), C56(H56), C66(H66), C9(H9), C55(H55), C64(H64), C28(H28),
 C17(H17), C54(H54), C49(H49), C30(H30), C21(H21), C31(H31), C65(H65), C41(H41),
  C40(H40), C42(H42), C45(H45), N15(H15), C18(H18A), C25(H25), C52(H52),
 C2(H2A), C50(H50), C24(H24A), C71(H71), C26(H26), C0AA(H0AA), C23(H23),
 C47(H47), C48(H48)
5.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C38(H38A,H38B,H38C), C62(H62A,H62B,H62C), C36(H36A,H36B,
 H36C), C60(H60A,H60B,H60C), C14(H14A,H14B,H14C), C76(H76A,H76B,H76C)
;
_olex2_submission_special_instructions 'No special instructions were received'