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_1556533
_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 S3, 3(B F4), B F3.5, 2(C2 H3 N)'
_chemical_formula_sum            'C64 H54 B4 F15.5 Fe2 N20 S3'
_chemical_formula_weight         1648.89
_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                95.29(3)
_cell_angle_beta                 100.29(3)
_cell_angle_gamma                92.93(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5210(19)
_cell_length_b                   16.723(3)
_cell_length_c                   23.621(5)
_cell_measurement_reflns_used    2499
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      2.27
_cell_volume                     3675.9(13)
_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(2)
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.900
_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  0.0971
_diffrn_reflns_av_unetI/netI     0.0898
_diffrn_reflns_Laue_measured_fraction_full 0.909
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            45853
_diffrn_reflns_point_group_measured_fraction_full 0.909
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         0.881
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       prism
_exptl_crystal_F_000             1675
_exptl_crystal_preparation       'Diethyl ether diffusion into acetonitrile'
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.0075
_exptl_crystal_size_min          0.0075
_refine_diff_density_max         1.472
_refine_diff_density_min         -1.550
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1047
_refine_ls_number_reflns         13521
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_gt           0.1086
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2905
_refine_ls_wR_factor_ref         0.3308
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8552
_reflns_number_total             13521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            FL273.cif
_cod_data_source_block           p-1_a
_cod_original_cell_volume        3675.8(13)
_cod_original_formula_sum        'C64 H54 B4 F15.50 Fe2 N20 S3'
_cod_database_code               1556533
_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. Shared sites
{B9, B9A}
3. Restrained distances
 F007-F006
 2.25 with sigma of 0.02
 F7AA-F2AA
 2.25 with sigma of 0.02
 F7AA-F1AA
 2.25 with sigma of 0.02
 F7AA-B2 = F2AA-B2 = F1AA-B2
 1.4 with sigma of 0.02
 B2-F1AA = B2-F2AA = B2-F7AA = B2-F0BA = B2-F1AB = B2-F5AA
 1.4 with sigma of 0.02
 B2A-F2AA = B2A-F7AA = B2A-F1AB = B2A-F5AA
 1.39 with sigma of 0.02
 B2-F1AA = B2-F2AA = B2-F0BA
 1.39 with sigma of 0.02
 F2AA-F1AA
 2.25 with sigma of 0.04
 F2AA-F7AA
 2.25 with sigma of 0.04
 F1AA-F0BA
 2.25 with sigma of 0.04
 F7AA-F0BA
 2.25 with sigma of 0.04
 F2AA-F0BA
 2.25 with sigma of 0.04
 F8-F10 \\sim F8-F11 \\sim F8-F15 \\sim F10-F11 \\sim F10-F15 \\sim F11-F15
 with sigma of 0.04
 B9-F8 \\sim B9-F10 \\sim B9-F11 \\sim B9-F15
 with sigma of 0.02
 F15-B9 \\sim F0AA-B9 \\sim F11-B9 \\sim F1-B9 \\sim F2-B9 \\sim F10-B9 \\sim
F4-B9 \\sim F8-B9
 with sigma of 0.02
 B9-F4 \\sim B9-F10 \\sim B9-F11 \\sim B9-F15 \\sim B9-F8 \\sim B9-F0AA \\sim
B9-F2 \\sim B9-F1
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C030) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(B9) = Uanis(B9A)
5. Rigid body (RIGU) restrains
 N02E, C02M, C02X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C030
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C030, C02V
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F3AA, F4AA, F6AA, F8AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, F2, F4, F0AA, B9, F8, F10, F11, F15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1AA, F2AA, F7AA, F0BA, B2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1AA, F2AA, F5AA, F7AA, F1AB, F0BA, B2, B2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, F2, F4, F0AA, B9, F8, F10, F11, F15, B9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F8, F10, F11, F15, B9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, F2, F4, F0AA, B9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: F1(0.5) F2(0.5) F4(0.5) F0AA(0.5) B9(0.5) F8(0.5) F10(0.5)
 F11(0.5) F15(0.5) B9A(0.5) F1AA(0.5) F5AA(0.5) F7AA(0.5) F1AB(0.5) F0BA(0.5)
 B2(0.5) B2A(0.5)
7.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), C3B(H3B), C5B(H5BA), C7B(H7B), C8B(H8B), C10B(H10B), C11B(H11B),
 C13B(H13B), C14B(H14B), C16B(H16B), C17B(H17B), C18B(H18B), C20B(H20B),
 C21B(H21B), C1C(H1C), C2C(H2CA), C4C(H4C), C6C(H6C), C7C(H7C), C9C(H9C),
 C10C(H10C), C12C(H12C), C13C(H13C), C15C(H15C), C16C(H16C), C17C(H17C),
 C19C(H19C), C20C(H20C)
7.b Idealised Me refined as rotating group:
 C030(H03A,H03B,H03C), C02X(H02A,H02B,H02C)
;
_olex2_exptl_crystal_mounting_method 'mounted with parafin oil'
_olex2_submission_special_instructions 'No special instructions were received'