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_7129112
_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_absolute_configuration rmad
_chemical_formula_moiety         'C126 H108 F6 Fe6 N32, 7(B F4)'
_chemical_formula_sum            'C126 H108 B7 F34 Fe6 N32'
_chemical_formula_weight         3127.21
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-03 deposited with the CCDC.	2021-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   26.679(3)
_cell_length_b                   26.679(3)
_cell_length_c                   21.8284(11)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    100
_cell_measurement_theta_max      22.6610
_cell_measurement_theta_min      1.4740
_cell_volume                     13455(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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   -145.00  24.00   1.00    0.20    --   30.00   0.00   0.00  169
  2  \f      0.00 179.00   1.00    0.20   0.00   0.00   0.00    --   179
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1039
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            84019
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         24.621
_diffrn_reflns_theta_min         1.480
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       block
_exptl_crystal_F_000             4755
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     960
_refine_ls_number_reflns         16361
_refine_ls_number_restraints     1155
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.1572
_refine_ls_R_factor_gt           0.0789
_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^)+(0.1610P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2135
_refine_ls_wR_factor_ref         0.2678
_reflns_Friedel_coverage         0.851
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                7658
_reflns_number_total             16361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04413c2.cif
_cod_data_source_block           m_ir_lt_020_a_88_1_col1_
_cod_depositor_comments
'Adding full bibliography for 7129106--7129112.cif.'
_cod_original_cell_volume        13455(3)
_cod_database_code               7129112
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.880
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51397
 0.48603
2. Restrained distances
 H36A-H41
 -2 with sigma of 0.02
 C19-C18 = C17-C16 = C25-C24
 1.54 with sigma of 0.02
 B6-F19 \\sim B6-F1A \\sim B6-F1B \\sim B6-F1C
 with sigma of 0.02
 B7-F1D \\sim B7-F1E \\sim B7-F1F \\sim B7-F1G
 with sigma of 0.02
 F1D-F1E \\sim F1E-F1F \\sim F1F-F1G \\sim F1G-F1D \\sim F1E-F1G \\sim F1D-F1F
 with sigma of 0.04
 F19-F1A \\sim F1A-F1B \\sim F1B-F1C \\sim F1C-F19 \\sim F1A-F1C \\sim F19-F1B
 with sigma of 0.04
 B4-F12 \\sim B4-F13 \\sim B4-F14 \\sim B4-F15
 with sigma of 0.02
 F12-F13 \\sim F13-F14 \\sim F14-F15 \\sim F15-F12 \\sim F13-F15 \\sim F12-F14
 with sigma of 0.04
 F16-F17 \\sim F17-F18 \\sim F18-F1H \\sim F1H-F16 \\sim F17-F1H \\sim F16-F18
 with sigma of 0.04
 B5-F16 \\sim B5-F17 \\sim B5-F18 \\sim B5-F1H
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
B6 \\sim F19 \\sim F1A \\sim F1B \\sim F1C: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
B7 \\sim F1D \\sim F1E \\sim F1F \\sim F1G: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
B4 \\sim F12 \\sim F13 \\sim F14 \\sim F15: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
B6 \\sim F19 \\sim F1A \\sim F1B \\sim F1C \\sim B4 \\sim F12 \\sim F14 \\sim
F15 \\sim F13: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
B5 \\sim F16 \\sim F17 \\sim F18 \\sim F1H: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
F18 \\sim B5 \\sim F16 \\sim F17 \\sim F1H: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C57 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004 within 2A
Uanis(F1F) \\sim Ueq, Uanis(B7) \\sim Ueq, Uanis(F1D) \\sim Ueq, Uanis(F1E)
\\sim Ueq, Uanis(F1G) \\sim Ueq: with sigma of 0.02 and sigma for terminal
atoms of 0.04
4. Rigid body (RIGU) restrains
 B7, F1D, F1E, F1F, F1G
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C36, Fe3, F1, N1, N3, Fe5, C3, C1, C9, C10, F3, F2, C2, C4, N2, C63, C11, C7,
 C5, C8, C62, C12, C6, C13, C23, N4, C22, Fe2, C21, N6, N10, N5, N9, N8, C20,
 C16, C15, C28, C27, C14, C48, C26, C25, C19, C17, C29, C44, C45, C47, C24, C18,
  N7, C43, C30, C46, C49, C31, C42, C61, C50, N11, C41, C60, N14, C32, C59, Fe4,
  C33, C51, N15, N12, N13, N16, C53, C34, C35, C58, C52, C54, C40, C37, C57,
 C55, C39, C38, C56
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B6, F19, F1A, F1B, F1C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B4, F12, F13, F14, F15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B5, F16, F17, F18, F1H
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(B4)=Sof(F12)=Sof(F13)=Sof(F14)=Sof(F15)=1-FVAR(1)
 Sof(B6)=Sof(F19)=Sof(F1A)=Sof(F1B)=Sof(F1C)=FVAR(1)
 Fixed Sof: B7(0.5) F1D(0.5) F1E(0.5) F1F(0.5) F1G(0.5)
6.a Riding coordinates:
 C58(H58A,H58B,H58C)
6.b Free rotating group:
 B6(F19,F1A,F1B,F1C), B4(F12,F13,F14,F15), B7(F1D,F1E,F1F,F1G), B5(F16,F17,F18,
 F1H)
6.c Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C24(H24A,H24B), C19(H19A,H19B), C18(H18A,H18B), C17(H17A,
 H17B), C25(H25A,H25B)
6.d Aromatic/amide H refined with riding coordinates:
 C31(H31), C63(H63), C43(H43), C44(H44), C10(H10), C62(H62), C42(H42),
 C50(H50), C28(H28), C5(H5), C13(H13), C15(H15), C4(H4), C41(H41), C22(H22),
 C7(H7), C23(H23), C60(H60), C20(H20), C40(H40), C48(H48), C6(H6), C45(H45),
 C26(H26), C37(H37), C54(H54), C38(H38), C39(H39), C46(H46), C61(H61), C55(H55),
  C56(H56), C57(H57)
6.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              36408
_shelx_hkl_checksum              79099
_shelx_fab_checksum              11133
_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
- B-factor correction
;