A large dinuclear Fe(ii) triple helicate demonstrating a two-step spin crossover.
Howard-Smith, Kyle J; Craze, Alexander R.; Zenno, Hikaru; Yagyu, Junya; Hayami, Shinya; Li, Feng; Chemical communications (Cambridge, England) 56 (2020) 8838–8841; doi:10.1039/d0cc03708g

data_7126792
_publ_section_title
;
 A large dinuclear Fe(ii) triple helicate demonstrating a two-step spin
 crossover.
;
_journal_issue                   62
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8838
_journal_page_last               8841
_journal_paper_doi               10.1039/d0cc03708g
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety
'C96 H65 Fe2 N12 O6 S6, 2(B F4), 2(B0.5 F2.1), 2.5(C2 H3 N), 2(B0.5 F1.8)'
_chemical_formula_sum            'C101 H72.5 B4 F15.8 Fe2 N14.5 O6 S6'
_chemical_formula_weight         2232.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-16 deposited with the CCDC.	2020-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.127(4)
_cell_length_b                   27.951(6)
_cell_length_c                   19.854(4)
_cell_measurement_reflns_used    7579
_cell_measurement_temperature    250
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      2.27
_cell_volume                     11169(4)
_computing_cell_refinement       XDS
_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      250
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'MX1 beamline Australian Synchrotron'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1096
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            141260
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.247
_diffrn_source
'silicon double crystal monochromated radiation'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.455
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       prism
_exptl_crystal_F_000             4553
_exptl_crystal_preparation
'To a stirring suspension of 0.35 mmol of L, an excess of Fe(II)BF4.6H2O (0.23 mmol) in 10 mL of acetonitrile was added dropwise at room temperature. The reaction mixture was then stirred and heated to reflux for 3 hours.'
_exptl_crystal_recrystallization_method 'Diethyl ether vapour diffusion.'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.256
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         11425
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.280
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0960
_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          0.2987
_refine_ls_wR_factor_ref         0.3219
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8179
_reflns_number_total             11425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03708g2.cif
_cod_data_source_block           fl665_250k_a
_cod_depositor_comments
'Adding full bibliography for 7126790--7126793.cif.'
_cod_original_formula_sum        'C101 H72.50 B4 F15.80 Fe2 N14.50 O6 S6'
_cod_database_code               7126792
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{B01T, B01U}
3. Restrained distances
 F00W-B01T \\sim F00X-B01U
 with sigma of 0.02
 F01C-B01T \\sim F0AA-B01U
 with sigma of 0.02
 F01P-B01T \\sim F01Q-B01U
 with sigma of 0.02
 B01T-F01W \\sim B01U-F01X
 with sigma of 0.02
 F00W-F01C \\sim F00X-F0AA
 with sigma of 0.04
 F00W-F01P \\sim F00X-F01Q
 with sigma of 0.04
 F00W-F01W \\sim F00X-F01X
 with sigma of 0.04
 F01C-F01P \\sim F0AA-F01Q
 with sigma of 0.04
 F01C-F01W \\sim F0AA-F01X
 with sigma of 0.04
 F01P-F01W \\sim F01Q-F01X
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C12 \\sim C021: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(B01T) = Uanis(B01U)
5. Rigid body (RIGU) restrains
 C11B, C12B, C13B, C14B, C15B, C16B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C01L, C01U
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F01D, F00F, F01J, F01O, B01Z
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B01T, F01C, F01P, F00W, F01W
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N023, C12, C021
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N023, C12, C021
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F0AA, F01Q, B01T, F00X, F01X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F01C, F01P, B01U, F00W, F01W
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: F00W(0.6) C5B(0.5) F01C(0.5) C11B(0.5) C16B(0.5) H01Y(0.5)
 C15B(0.5) H01X(0.5) C14B(0.5) C13B(0.5) H01R(0.5) C12B(0.5) H01V(0.5) O1B(0.5)
 F01P(0.5) C8B(0.5) B01T(0.5) F01W(0.5) C021(0.25) C6B(0.5) H022(0.5)
 N023(0.25) C7B(0.5) H024(0.5) C12(0.25) H12A(0.25) H12B(0.25) H12C(0.25)
 C01W(0.5) H01W(0.5) C9B1(0.5) C10B(0.5) H01Z(0.5) C1(0.5) H1AA(0.5) C2(0.5)
 C3(0.5) O1B1(0.5) C5B1(0.5) H00U(0.5) H00A(0.5) H01B(0.5) H01A(0.5) C8B1(0.5)
 C7B1(0.5) H2(0.5) C6B1(0.5) H1(0.5) F01X(0.5) F01Q(0.5) B01U(0.5) F0AA(0.5)
 F00X(0.3)
7.a Aromatic/amide H refined with riding coordinates:
 C4B(H00I), C18A(H00J), C6A(H00K), C13A(H00L), C7A(H00M), C21A(H00O),
 C22A(H00Q), C12A(H00R), C15A(H00T), C19A(H00V), C4A(H00Y), C10A(H00Z),
 C16A(H012), C9A(H013), C29A(H014), C1A(H015), C24A(H016), C1B(H017),
 C25A(H019), C2B(H01E), C27A(H01F), C16B(H01Y), C15B(H01X), C13B(H01R),
 C12B(H01V), C28A(H01I), C32A(H01K), C31A(H01M), C2A(H01N), C6B(H022),
 C7B(H024), C01W(H01W), C10B(H01Z), C1(H1AA), C4(H00U), C4(H00A), C9B(H01B),
 C9B(H01A), C7B1(H2), C6B1(H1)
7.b Fitted hexagon refined as free rotating group:
 C11B(C16B,C15B,C14B,C13B,C12B), C01W(C9B1,C10B,C1,C2,C3), C5B1(C4,C9B,C8B1,
 C7B1,C6B1)
7.c Idealised Me refined as rotating group:
 C01U(H01C,H01D,H01G), C12(H12A,H12B,H12C)
;
_olex2_exptl_crystal_mounting_method
'Cold mounted in a CO2 atmosphere, uisng cryotox oil. '
_olex2_submission_special_instructions 'No special instructions were received'