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_1556532
_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
;
C63 H54 Fe2 N18, 2(B0.4 F0.8), 2(B F4), 
2(B0.6 F3.2), 2(C0.5 H0.75 N0.5), 0.5(C2 H3 N)
;
_chemical_formula_sum            'C65 H57 B4 F16 Fe2 N19.5'
_chemical_formula_weight         1570.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 107.00(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.131(4)
_cell_length_b                   17.391(4)
_cell_length_c                   21.069(4)
_cell_measurement_reflns_used    2494
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      2.26
_cell_volume                     7404(3)
_computing_cell_refinement       'ShelXL least squares'
_computing_data_collection       XDS
_computing_data_reduction        xprep
_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      293(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.917
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            50460
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         1.545
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       needle
_exptl_crystal_F_000             3198
_exptl_crystal_recrystallization_method
'diethyl ether vapour 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         1.371
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         6995
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      1.416
_refine_ls_R_factor_all          0.1371
_refine_ls_R_factor_gt           0.1035
_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^)+(0.1280P)^2^+69.2223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2930
_refine_ls_wR_factor_ref         0.3220
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4686
_reflns_number_total             6995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            FL206_a.cif
_cod_data_source_block           fl206_a
_cod_original_formula_sum        'C65 H57 B4 F16 Fe2 N19.50'
_cod_database_code               1556532
_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. Shared sites
{B01C, B01B}
3. Restrained distances
 B01B-B01C
 1.42 with sigma of 0.02
 F00X-B01B = F00Y-B01C = F3-B01B = F009-B01C = F10-B01B = F00T-B01C = F00H-
 B01C = F1-B01B
 1.39 with sigma of 0.02
 C1-C2 \\sim C11A-C2
 with sigma of 0.02
4. Rigid bond restraints
 C3B', C4C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(B01C) = Uanis(B01B)
6. Rigid body (RIGU) restrains
 N1B, N2B, N1B', N2B', C1B, C2B, C3B, C1B', C2B', C3B'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F009, F00H, F00T, F00Y
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C2, C5, C6, C7, C8, C11A, C12A, C13A, C14A, C15A, C16A, C17A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C15A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9, C5A, C6A, C7A, C8A, C9A, C10A, C5A', C6A', C7A', C8A', C9A'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4B, C4C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: N1B(0.5) N2B(0.5) H2B(0.5) N1B'(0.5) N2B'(0.5) H2B'(0.5) C1(0.5)
 H1A(0.5) H1B(0.5) C3(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5) C12A(0.5) C7(0.5)
 H7(0.5) C8(0.5) H8(0.5) C7A(0.5) H7A(0.5) C8A(0.5) C9A(0.5) H9A(0.5) C9(0.5)
 H9(0.5) C5A(0.5) C6A(0.5) H6A(0.5) C11A(0.5) H11A(0.5) H11B(0.5) C15A(0.5)
 C16A(0.5) H16A(0.5) C17A(0.5) H17A(0.5) C2(0.5) C13A(0.5) H13A(0.5) C14A(0.5)
 H14A(0.5) C7A'(0.5) H7A'(0.5) C8A'(0.5) C9A'(0.5) H9A'(0.5) C10A(0.5)
 H10A(0.5) C5A'(0.5) C6A'(0.5) H6A'(0.5) C1B(0.5) H1BA(0.5) C2B(0.5) H2BA(0.5)
 C3B(0.5) C4B(0.5) H4B(0.5) H11C(0.5) H11D(0.5) C1B'(0.5) H1B'(0.5) C2B'(0.5)
 H2BB(0.5) C3B'(0.5) C4C(0.5) H4C(0.5) F1(0.2) F3(0.2) F10(0.2) F00X(0.2)
 B01B(0.4) F009(0.8) F00H(0.8) F00T(0.8) F00Y(0.8) B01C(0.6) N2(0.5) C1AA(0.25)
 C2AA(0.25) H2AB(0.25) H2AC(0.25) H2AD(0.25) N01L(0.25) C4(0.25) H4D(0.25)
 H4E(0.25) H4F(0.25) C0AA(0.25)
8.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C11A(H11A,H11B), C11B(H11C,H11D)
8.b Aromatic/amide H refined with riding coordinates:
 N2A(H2A), N5A(H5A), N2B(H2B), N2B'(H2B'), C5(H5), C6(H6), C7(H7), C8(H8),
 C1A(H1AA), C2A(H2AA), C4A(H4A), C7A(H7A), C9A(H9A), C9(H9), C6A(H6A),
 C16A(H16A), C17A(H17A), C13A(H13A), C14A(H14A), C18A(H18A), C20A(H20A),
 C21A(H21A), C7A'(H7A'), C9A'(H9A'), C10A(H10A), C6A'(H6A'), C1B(H1BA),
 C2B(H2BA), C4B(H4B), C6B(H6B), C7B(H7B), C9B(H9B), C10B(H10B), C1B'(H1B'),
 C2B'(H2BB), C4C(H4C)
8.c Fitted hexagon refined as free rotating group:
 C3(C5,C6,C12A,C7,C8), C7A(C8A,C9A,C9,C5A,C6A), C15A(C16A,C17A,C2,C13A,C14A),
 C7A'(C8A',C9A',C10A,C5A',C6A')
8.d Idealised Me refined as rotating group:
 C2AA(H2AB,H2AC,H2AD), C4(H4D,H4E,H4F)
;
_olex2_exptl_crystal_mounting_method 'mounted in parafin oil'
_olex2_submission_special_instructions 'No special instructions were received'