Investigation of the Spin Crossover Properties of Three Dinulear Fe(II) Triple Helicates by Variation of the Steric Nature of the Ligand Type
Craze, A.R.; Sciortino, N.F.; Badbhade, M.M.; Kepert, C.J.; Marjo, C.E.; Li, F.; Inorganics 5 (2017) 62–; doi:10.3390/inorganics5040062

data_1556531
_publ_section_title
;
 Investigation of the Spin Crossover Properties of Three Dinulear Fe(II)
 Triple Helicates by Variation of the Steric Nature of the Ligand Type
;
_journal_name_full               Inorganics
_journal_page_first              62
_journal_paper_doi               10.3390/inorganics5040062
_journal_volume                  5
_journal_year                    2017
_chemical_formula_moiety         'C60 H48 Fe2 N18 O3, 2(C2 H3 N), 4(B F4)'
_chemical_formula_sum            'C64 H54 B4 F16 Fe2 N20 O3'
_chemical_formula_weight         1610.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                77.43(3)
_cell_angle_beta                 77.58(3)
_cell_angle_gamma                86.73(3)
_cell_formula_units_Z            2
_cell_length_a                   13.837(3)
_cell_length_b                   13.855(3)
_cell_length_c                   20.684(4)
_cell_measurement_reflns_used    2569
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      2.26
_cell_volume                     3779.5(15)
_computing_cell_refinement       'ShelXL least squares'
_computing_data_collection       XDS
_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      100
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.909
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            57096
_diffrn_reflns_point_group_measured_fraction_full 0.909
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.031
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       needle
_exptl_crystal_F_000             1636
_exptl_crystal_recrystallization_method
'Diethyl ether diffusion into acetonitrile'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.212
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1095
_refine_ls_number_reflns         14860
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1071P)^2^+7.1169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1966
_refine_ls_wR_factor_ref         0.2111
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11524
_reflns_number_total             14860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            FL204_a.cif
_cod_data_source_block           fl204_a
_cod_database_code               1556531
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.990
_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. Rigid bond restraints
 C5E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C7D) = Uanis(C6D)
4. Rigid body (RIGU) restrains
 N3, C1AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N031
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N02Y
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2AA, C0AA, N0AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C2, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, C5, N4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N0AA, C0AA, C2AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N0AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8C, C9C, C4AA, C3AA, C10C, C5E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N5B(0.5) H5B(0.5) N6B(0.5) H17C(0.5) H17B(0.5) C18B(0.5) C19B(0.5)
 H19B(0.5) C20B(0.5) H20B(0.5) C4AA(0.5) H4AA(0.5) C3AA(0.5) H3AA(0.5) C9C(0.5)
 H9C(0.5) C10C(0.5) H10C(0.5) C1(0.5) H1D(0.5) H1E(0.5) H1F(0.5) C1AA(0.5)
 N3(0.5) N031(0.5) C02S(0.5) H02A(0.5) H02B(0.5) H02C(0.5) C02W(0.5) N02Y(0.5)
 C02X(0.5) H02D(0.5) H02E(0.5) H02F(0.5) C02Z(0.5) C2(0.25) H2D(0.25) H2E(0.25)
 H2F(0.25) N4(0.25) C5(0.25) N0AA(0.25) C0AA(0.25) C2AA(0.25) H2AC(0.25)
 H2AD(0.25) H2AE(0.25) N1AA(0.5) C5AA(0.5) H5AA(0.5) N2AA(0.5) H2AB(0.5)
 C6AA(0.5) H6AA(0.5) C7AA(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 N2A(H2A), N5A(H5A), N2B(H2B), N5B(H5B), N2C(H2C), N5C(H5C), C1A(H1A),
 C2A(H2AA), 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(H2BA), C4B(H4B), C6B(H6B), C7B(H7B), C9B(H9B), C10B(H10B),
 C12B(H12B), C13B(H13B), C15B(H15B), C16B(H16B), C17B(H17C), C17B(H17B),
 C19B(H19B), C20B(H20B), C1C(H1C), C2C(H2CA), C4C(H4C), C4AA(H4AA), C3AA(H3AA),
 C9C(H9C), C10C(H10C), C12C(H12C), C13C(H13C), C15C(H15C), C16C(H16C),
 C17C(H17D), C19C(H19C), C20C(H20C), C5AA(H5AA), N2AA(H2AB), C6AA(H6AA),
 C7D(H7D), C6D(H6D)
6.b Idealised Me refined as rotating group:
 C1(H1D,H1E,H1F), C02S(H02A,H02B,H02C), C02X(H02D,H02E,H02F), C2(H2D,H2E,H2F),
 C2AA(H2AC,H2AD,H2AE)
;
_olex2_exptl_crystal_mounting_method 'room temperature in parafin oil'
_olex2_submission_special_instructions 'No special instructions were received'