Self-assembly of a trigonal bipyramidal architecture with stabilisation of iron in three spin states.
Taylor, Lauren L. K.; Vitorica-Yrezabal, Iñigo J; Borilović, Ivana; Tuna, Floriana; Riddell, Imogen A.; Chemical communications (Cambridge, England) 57 (2021) 11252–11255; doi:10.1039/d1cc04413c

data_7129107
_publ_section_title
;
 Self-assembly of a trigonal bipyramidal architecture with stabilisation
 of iron in three spin states.
;
_journal_issue                   85
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11252
_journal_page_last               11255
_journal_paper_doi               10.1039/d1cc04413c
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'C58 H43.5 Fe N12.5 O3, B F4, B F3.84, C1.9 H3 N0.72, 0.86(C2 H3 N1)'
_chemical_formula_sum            'C61.62 H49.07 B2 F7.84 Fe N14.07 O3'
_chemical_formula_weight         1261.14
_chemical_name_systematic        IR-LT-020(3L1M)
_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
_audit_creation_date             2019-08-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-09 deposited with the CCDC.	2021-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                71.694(5)
_cell_angle_beta                 81.751(5)
_cell_angle_gamma                70.445(6)
_cell_formula_units_Z            2
_cell_length_a                   10.5589(7)
_cell_length_b                   14.5471(9)
_cell_length_c                   21.5140(12)
_cell_measurement_reflns_used    5573
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      25.4390
_cell_measurement_theta_min      1.9650
_cell_volume                     2953.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_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_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.732
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -80.00  96.00   1.00    8.00    --    7.40  30.00-180.00  176
  2  \w    -80.00  16.00   1.00    8.00    --    7.40  60.00-120.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0844
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.732
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24792
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.732
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.479
_diffrn_reflns_theta_min         1.996
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.42a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_preparation
'diffusion of diethyl ether into acetonitrile'
_exptl_crystal_recrystallization_method
'diffusion of diethyl ether into acetonitrile'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.262
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     877
_refine_ls_number_reflns         13157
_refine_ls_number_restraints     448
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1325
_refine_ls_R_factor_gt           0.0896
_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^)+(0.1349P)^2^+3.5102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2300
_refine_ls_wR_factor_ref         0.2558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8895
_reflns_number_total             13157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04413c2.cif
_cod_data_source_block           lir2
_cod_depositor_comments
'Adding full bibliography for 7129106--7129112.cif.'
_cod_original_cell_volume        2953.7(4)
_cod_database_code               7129107
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.967
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9BA-C8BA = C3BA-C3 = C3A-C1A = C2_$1-C1_$1
 1.46 with sigma of 0.001
 N1AB-C3A = N4AA-C3 = N2AA-C9BA = N1AA_$1-C1_$1
 1.16 with sigma of 0.01
 C3BA-C3
 1.45 with sigma of 0.02
 C3A-C1A = C3BA-C3 = C9BA-C8BA = C2_$1-C1_$1
 1.45 with sigma of 0.02
 O2-C5BA
 1.2 with sigma of 0.001
 N1AB_$2-O2
 -3 with sigma of 0.02
 C3BA-C3 \\sim C1A-C3A
 with sigma of 0.02
 C19-C5BA \\sim C5BA-N3BA
 with sigma of 0.001
 C62-C70 \\sim C62-C70A
 with sigma of 0.02
 C12-C19 \\sim C12A-C19A
 with sigma of 0.02
 C12-N3BA \\sim C12A-N3BB
 with sigma of 0.02
 C12-C5BA \\sim C12A-C5BB
 with sigma of 0.02
 C19-C88 \\sim C19A-C88A
 with sigma of 0.02
 C88-C70 \\sim C88A-C70A
 with sigma of 0.02
 C70-C68 \\sim C70A-C68A
 with sigma of 0.02
 C68-N3BA \\sim C68A-N3BB
 with sigma of 0.02
 C5BA-O2 \\sim C5BB-O2A
 with sigma of 0.02
 C62-C88 \\sim C62-C88A
 with sigma of 0.04
 C62-C68 \\sim C62-C68A
 with sigma of 0.04
 C12-C88 \\sim C12A-C88A
 with sigma of 0.04
 C12-C68 \\sim C12A-C68A
 with sigma of 0.04
 C12-O2 \\sim C12A-O2A
 with sigma of 0.04
 C19-C70 \\sim C19A-C70A
 with sigma of 0.04
 C19-N3BA \\sim C19A-N3BB
 with sigma of 0.04
 C19-C5BA \\sim C19A-C5BB
 with sigma of 0.04
 C88-C68 \\sim C88A-C68A
 with sigma of 0.04
 C70-N3BA \\sim C70A-N3BB
 with sigma of 0.04
 N3BA-C5BA \\sim N3BB-C5BB
 with sigma of 0.04
 C70A-C62 \\sim C70-C62
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N3BA \\sim C70 \\sim C88 \\sim C68 \\sim C19 \\sim C12: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002
C5BA \\sim C12 \\sim C19 \\sim N3BA: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C70 \\sim C68 \\sim C88 \\sim C12 \\sim N3BA \\sim C19 \\sim C5BA \\sim O2:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C3BA \\sim C3A \\sim C3 \\sim N4AA \\sim N1AB \\sim C1A: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
N1AB \\sim N4AA \\sim C3 \\sim C3A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C12 \\sim C19 \\sim C88 \\sim C70 \\sim C68 \\sim N3BA \\sim C70A \\sim C88A
\\sim C19A \\sim C12A \\sim N3BB \\sim C68A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C5BA \\sim O2 \\sim C5BB \\sim O2A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O2A \\sim O2: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C12, C19, C88, C70, C68, N3BA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C68, C70, C88, C19, C12, C62, C75
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1AB, C3A, C1A, C3BA, C3, N4AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C19, C88, C70, C68, N3BA, C5BA, O2, C70A, C19A, C12A, C5BB, O2A, N3BB,
 C68A, C88A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F4AA)=Sof(F5AA)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(C3BA)=Sof(H3BA)=Sof(H3BB)=Sof(H3BC)=Sof(N4AA)=Sof(C3)=FVAR(2)
 Sof(C70A)=Sof(C88A)=Sof(H88A)=Sof(C19A)=Sof(H19A)=Sof(C12A)=Sof(C5BB)=
 Sof(H5BB)=Sof(O2A)=Sof(N3BB)=Sof(C68A)=Sof(H68A)=1-FVAR(3)
 Sof(C12)=Sof(C19)=Sof(H19)=Sof(C88)=Sof(H88)=Sof(C70)=Sof(C68)=Sof(H68)=
 Sof(N3BA)=Sof(C5BA)=Sof(H5BA)=Sof(O2)=FVAR(3)
 Fixed Sof: C1A(0.25) H1AA(0.25) H1AB(0.25) H1AC(0.25) C3A(0.25) N1AB(0.25)
 C1(0.5) N1AA(0.5) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5)
6.a Me refined with riding coordinates:
 C4BA(H4BA,H4BB,H4BC), C9AA(H9AA,H9AB,H9AC), C7BA(H7BA,H7BB,H7BC), C2(H2A,H2B,
 H2C)
6.b Aromatic/amide H refined with riding coordinates:
 C44(H44), C58(H58), C40(H40), C29(H29), C33(H33), C36(H36), C42(H42),
 C43(H43), C56(H56), C53(H53), C63(H63), C32(H32), C59(H59), C64(H64), C87(H87),
  C71(H71), C60(H60), C55(H55), C19(H19), C88(H88), C68(H68), C69(H69),
 C75(H75), C79(H79), C4AA(H4AA), C1BA(H1BA), C15(H15), C0BA(H0BA), C7AA(H7AA),
 C13(H13), C6AA(H6AA), C11(H11), C5BA(H5BA), C88A(H88A), C19A(H19A), C5BB(H5BB),
  C68A(H68A)
6.c Fitted hexagon refined as free rotating group:
 N11(C25,C44,C58,C38,C40), C57(C2BA,C56,C53,C63,C32), C67(C87,C71,C60,C55,C41),
  C12(C19,C88,C70,C68,N3BA), C4AA(C1BA,C15,C0BA,C2AA,C0AA)
6.d Idealised Me refined as rotating group:
 C8BA(H8BA,H8BB,H8BC), C3BA(H3BA,H3BB,H3BC), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              54914
_shelx_hkl_checksum              7249
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;