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_7129110
_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         'C126 H108 F6 Fe6 N32, 7(B F4)'
_chemical_formula_sum            'C126 H108 B7 F34 Fe6 N32'
_chemical_formula_weight         3127.21
_chemical_name_systematic        IR-LT-020(9.28)
_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   geom
_audit_creation_date             2019-04-25
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   26.433(2)
_cell_length_b                   26.433(2)
_cell_length_c                   22.1827(13)
_cell_measurement_reflns_used    6530
_cell_measurement_temperature    100
_cell_measurement_theta_max      15.8890
_cell_measurement_theta_min      1.7160
_cell_volume                     13422.6(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14d (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14d (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14d (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.388
_diffrn_measured_fraction_theta_max 0.998
_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       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.388
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43352
_diffrn_reflns_point_group_measured_fraction_full 0.379
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         17.424
_diffrn_reflns_theta_min         1.724
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.02496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14d (Rigaku Oxford Diffraction, 2018)
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    1.161
_exptl_crystal_description       block
_exptl_crystal_F_000             4755
_exptl_crystal_preparation       'Made in acetonitrile'
_exptl_crystal_recrystallization_method
'diffusion of diethyl ether into acetonitrile solution'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.54(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.277
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         6133
_refine_ls_number_restraints     1197
_refine_ls_restrained_S_all      1.578
_refine_ls_R_factor_all          0.1397
_refine_ls_R_factor_gt           0.1094
_refine_ls_shift/su_max          0.002
_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         0.3273
_reflns_Friedel_coverage         0.826
_reflns_Friedel_fraction_full    0.368
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3912
_reflns_number_total             6133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04413c2.cif
_cod_data_source_block           m_ir_lt_020_928_c_col1_
_cod_depositor_comments
'Adding full bibliography for 7129106--7129112.cif.'
_cod_original_cell_volume        13423(2)
_cod_database_code               7129110
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.897
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49(8)
 0.51(8)
2. 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
3. Restrained distances
 N01Q_$1-C9_$1
 1.603 with sigma of 0.02
 N36-C44 = N01Q-C8
 1.479 with sigma of 0.02
 N009_$2-N8AA_$2 = N9-N0AA
 2.065 with sigma of 0.02
 N0AA-C59 = N9-C58
 1.363 with sigma of 0.02
 N9-C56 = N0AA-C56 = N0AA-C59 = N9-C58 = N007-C23 = N007-C20 = N00Q-C20 = N00Q-
 C22 = N009-C35 = N009-C38 = N8AA-C37 = N8AA-C35
 1.363 with sigma of 0.02
 N9-C57
 1.479 with sigma of 0.002
 C4-C3 = C2-C3 = C2-C1
 1.4 with sigma of 0.002
 N009-C33
 2.63 with sigma of 0.02
 N00V-C3
 2.63 with sigma of 0.02
 N00V-C4
 1.585 with sigma of 0.002
 C4-C3
 1.21 with sigma of 0.002
 C3-C1
 2.408 with sigma of 0.002
 N00B-C3
 1.39 with sigma of 0.002
 N00B-C2
 2.408 with sigma of 0.002
 F19-B4 = F17-B4 = F18-B4 = F16-B4
 1.43 with sigma of 0.002
 F6-B1 = F5-B1 = F4-B1 = F7-B1
 1.43 with sigma of 0.002
 N26-C5
 2.4 with sigma of 0.02
 F13-F15
 2.33 with sigma of 0.02
 F16-F19
 2.33 with sigma of 0.02
 F9-F8
 2.33 with sigma of 0.02
 F8-F11
 2.33 with sigma of 0.02
 F14-F15
 2.33 with sigma of 0.02
 F18-F19
 2.33 with sigma of 0.02
 F17-F19
 2.33 with sigma of 0.02
 C45-C44
 2.4 with sigma of 0.02
 N00Q-C21
 1.45 with sigma of 0.002
 C8-N26
 2.4 with sigma of 0.002
 C51-C49
 1.5 with sigma of 0.01
 C7-C8 = C43-C44
 1.54 with sigma of 0.02
 N26-C7 = N26-C43 = N26-C6
 1.522 with sigma of 0.002
 C7-C6
 2.4 with sigma of 0.02
 N00V-C6
 2.4 with sigma of 0.02
 H7A-H6B
 -2 with sigma of 0.02
 C43-C6
 2.6 with sigma of 0.01
 C6-C7
 2.6 with sigma of 0.01
 C7-C43
 2.6 with sigma of 0.01
 F15-B3 = F14-B3 = F13-B3 = F12-B3
 1.43 with sigma of 0.002
 F9-B2 = F8-B2 = F11-B2 = F10-B2
 1.43 with sigma of 0.002
 F10-F11
 2.33 with sigma of 0.02
 F9-F10
 2.33 with sigma of 0.02
 F10-F8
 2.33 with sigma of 0.02
 F12-F15
 2.33 with sigma of 0.02
 F14-F13 = F12-F13 = F14-F12 = F14-F15 = F13-F15 = F12-F15 = F17-F16 = F16-F19
 = F17-F19 = F17-F18 = F19-F18 = F16-F18
 2.335 with sigma of 0.001
 F10-F12
 -2.5 with sigma of 0.01
 C20_$1-C23_$1 \\sim N007_$1-C22_$1 \\sim N00Q_$1-C23_$1 \\sim C22_$1-C20_$1
\\sim N00Q_$1-
 N007_$1
 with sigma of 0.02
 N007_$1-C20_$1 \\sim N00Q_$1-C20_$1
 with sigma of 0.02
 N009-C37 \\sim N8AA-C38 \\sim C35-C38 \\sim N8AA-N009 \\sim C37-C35 \\sim
C20-C23 \\sim N00Q-N007 ~
 N00Q-C23 \\sim N007-C22 \\sim C22-C20
 with sigma of 0.02
 C56-C58 \\sim N9-N0AA \\sim C56-C59 \\sim N0AA-C58 \\sim N9-C59
 with sigma of 0.02
 C58-C57 \\sim C57-C56
 with sigma of 0.002
 C16-C13 \\sim C13-C19
 with sigma of 0.01
 C12-C15 \\sim C15-C14
 with sigma of 0.01
 F5-F7 \\sim F6-F5 \\sim F6-F7 \\sim F6-F4 \\sim F7-F4 \\sim F5-F4
 with sigma of 0.002
 C6-C5 \\sim C7-C8 \\sim C43-C44
 with sigma of 0.002
 N26-C7 \\sim N26-C43 \\sim N26-C6 \\sim N00V-C5 \\sim N36-C44 \\sim N01Q-C8
 with sigma of 0.002
 N26-C7 \\sim N26-C6 \\sim N26-C43
 with sigma of 0.002
 C43-C44 \\sim C6-C5 \\sim C7-C8
 with sigma of 0.002
 N00V-C5 \\sim N36-C44 \\sim N01Q-C8 \\sim N26-C6 \\sim N26-C43 \\sim N26-C7
 with sigma of 0.002
 C7-C8 \\sim C43-C44 \\sim C6-C5
 with sigma of 0.002
4. Restrained planarity
 C57, N9, C56, N0AA, C59, C58
 with sigma of 0.1
 N00B, C1, C3, C2
 with sigma of 0.1
 C36, N8AA, C37, C38, N009, C35
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C52 \\sim C51 \\sim C55 \\sim C54 \\sim N16 \\sim C53 \\sim C56 \\sim N9 \\sim
C57 \\sim N0AA \\sim C58 \\sim C59: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
B4 \\sim F18 \\sim F16 \\sim F19 \\sim F17: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
F6 \\sim F5 \\sim B1 \\sim F7 \\sim F4: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C6 \\sim N26 \\sim C7 \\sim C43: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C5 \\sim C6 \\sim C7 \\sim C8 \\sim C44 \\sim N26 \\sim C43 \\sim N00V: within
2A with sigma of 0.002 and sigma for terminal atoms of 0.004
B2 \\sim F10 \\sim F11 \\sim F9 \\sim F8: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
B3 \\sim F15 \\sim F13 \\sim F12 \\sim F14: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C26 \\sim C25 \\sim C27 \\sim C22 \\sim C23 \\sim C24: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 N26, C6, C44, C43, C7
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N26, Fe2, N00J, F1, C34, C33, Fe3, C30, C35, C32, F3, F2, C29, C31, N009,
 N8AA, Fe4, C28, C38, C36, C37, N007, N00K, C39, C42, C20, C23, C19, C18, C40,
 C41, N00Q, C24, C22, C15, C17, C21, C25, C27, C16, C13, C26, C14, C12, N00H,
 C11, Fe1, C10, N00B, N00V, N9BA, N01Q, N36, C9, C3, C4, C5, C46, C50, C8, C45,
 C44, C2, C6, C47, C49, C7, C43, C1, C48, C51, C52, C55, C53, N16, C54, C56,
 N0AA, N9, C59, C58, C57, C60, C63, C61, C62
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
7. Others
 Fixed Sof: F5(0.5) F7(0.5) B1(0.5) F6(0.5) F4(0.5)
8.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C8(H8A,H8B), C43(H43A,H43B), C7(H7A,H7B), C5(H5A,H5B), C6(H6A,
 H6B)
8.b Me refined with riding coordinates:
 C36(H36A,H36B,H36C), C21(H21A,H21B,H21C), C57(H57A,H57B,H57C)
8.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C16(H16), C17(H17), C1(H1), C14(H14), C12(H12), C11(H11), C28(H28),
 C47(H47), C48(H48), C50(H50), C31(H31), C34(H34), C32(H32), C52(H52), C53(H53),
  C55(H55), C9(H9), C63(H63), C62(H62), C61(H61), C60(H60), C41(H41), C42(H42),
 C39(H39), C40(H40), C2(H2), C25(H25), C24(H24), C27(H27), C26(H26), C45(H45),
 C4(H4)
8.d Fitted hexagon refined as free rotating group:
 N00K(C19,C15,C16,C17,C18), C14(C13,C12,C11,C10,N00H), C46(C47,C48,C49,C50,
 N9BA), C31(C30,C34,N00J,C33,C32), C52(C53,C54,N16,C55,C51), C58(C63,C62,C61,
 C60,C59), C41(C42,C37,C38,C39,C40), C25(C24,C23,C22,C27,C26)
;
_shelx_res_checksum              66260
_shelx_hkl_checksum              78712
_shelx_fab_checksum              43289
_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
;