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_7129109
_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         'C63 H54 Fe N16, 2(B F4)'
_chemical_formula_sum            'C63 H54 B2 F8 Fe N16'
_chemical_formula_weight         1264.69
_chemical_name_systematic        1
_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
_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                73.976(13)
_cell_angle_beta                 70.124(14)
_cell_angle_gamma                60.931(19)
_cell_formula_units_Z            2
_cell_length_a                   15.105(3)
_cell_length_b                   15.136(2)
_cell_length_c                   19.131(3)
_cell_measurement_reflns_used    2469
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      48.8030
_cell_measurement_theta_min      3.3780
_cell_volume                     3562.4(12)
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.954
_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    -25.00   2.00   1.00   20.00    --    5.00  57.00-180.00   27
  2  \w    -85.00  13.00   1.00   20.00    --  -44.70  76.00 -90.00   98
  3  \w    -64.00  28.00   1.00   20.00    --  -44.70  57.00 120.00   92
  4  \w    -63.00  29.00   1.00   20.00    --  -44.70  57.00  60.00   92
  5  \w    -77.00  21.00   1.00   20.00    --  -44.70  76.00 -30.00   98
  6  \w    -77.00  20.00   1.00   20.00    --  -44.70  57.00-150.00   97
  7  \w    -63.00 -27.00   1.00   20.00    -- -110.00  76.00   0.00   36
  8  \w   -126.00 -98.00   1.00   20.00    -- -110.00  76.00   0.00   28
  9  \w   -149.00 -22.00   1.00   20.00    -- -110.00  76.00 120.00  127
 10  \w   -173.00 -79.00   1.00   20.00    -- -110.00 -57.00 150.00   94
 11  \w   -193.00 -70.00   1.00   20.00    -- -110.00 -38.00  60.00  123
 12  \w   -121.00 -93.00   1.00   20.00    -- -110.00  76.00-180.00   28
 13  \w   -103.00 -76.00   1.00   20.00    -- -110.00  76.00 -30.00   27
 14  \w    -72.00 -38.00   1.00   20.00    -- -110.00  76.00 -30.00   34
 15  \w    -62.00 -37.00   1.00   20.00    -- -110.00  76.00  30.00   25
 16  \w   -124.00 -80.00   1.00   20.00    -- -110.00  76.00  30.00   44
 17  \w   -198.00-123.00   1.00   20.00    -- -110.00 -57.00-180.00   75
 18  \w   -124.00 -82.00   1.00   20.00    -- -110.00  76.00-150.00   42
 19  \w   -132.00 -40.00   1.00   20.00    -- -110.00  76.00  60.00   92
 20  \w   -148.00 -22.00   1.00   20.00    -- -110.00  76.00 -90.00  126
 21  \w   -108.00 -52.00   1.00   20.00    -- -110.00  76.00 150.00   56
 22  \w   -105.00 -78.00   1.00   20.00    -- -110.00  76.00  90.00   27
 23  \w   -188.00 -69.00   1.00   20.00    -- -110.00 -38.00  30.00  119
 24  \w   -107.00 -21.00   1.00   20.00    -- -110.00  57.00 -90.00   86
 25  \w    -74.00 -47.00   1.00   20.00    -- -110.00   0.00-120.00   27
 26  \w   -136.00-105.00   1.00   20.00    -- -110.00   0.00-120.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1226
_diffrn_reflns_av_unetI/netI     0.1357
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40026
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.798
_diffrn_reflns_theta_min         2.478
_exptl_absorpt_coefficient_mu    2.276
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89700
_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 light violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       plate
_exptl_crystal_F_000             1304
_exptl_crystal_preparation       'Made in acetonitrile'
_exptl_crystal_recrystallization_method
'Diffusion of diethyl ether into acetonitrile'
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         14501
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1780
_refine_ls_R_factor_gt           0.0955
_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^)+(0.1717P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2538
_refine_ls_wR_factor_ref         0.3085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6112
_reflns_number_total             14501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04413c2.cif
_cod_data_source_block           rir3
_cod_depositor_comments
'Adding full bibliography for 7129106--7129112.cif.'
_cod_original_cell_volume        3562.6(12)
_cod_database_code               7129109
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.935
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H35(0.065) H36(0.068) H38(0.058) H33(0.069) H30(0.068) H31(0.069)
 H44(0.065) H39(0.063) H1A(0.071) H1B(0.071) H41A(0.071) H41B(0.071) H3(0.067)
 H2A(0.067) H2B(0.067) H40A(0.067) H40B(0.067) H47(0.079) H46(0.079) H49(0.066)
 H43A(0.066) H43B(0.066) H42A(0.074) H42B(0.074) H60(0.077) H59(0.085)
 H58(0.094) H61(0.07) H11(0.086) H10(0.084) H13(0.087) H52(0.082) H51(0.08)
 H54(0.083) H26(0.077) H6(0.092) H8(0.061) H5(0.079) H17(0.121) H18(0.088)
 H19(0.07) H20(0.067) H25(0.109) H23(0.153) H24(0.159) H56A(0.194) H56B(0.194)
 H56C(0.194) H21A(0.218) H21B(0.218) H21C(0.218) H15A(0.355) H15B(0.355)
 H15C(0.355)
 Fixed X: H35(0.374319) H36(0.392559) H38(0.66258) H33(0.660867) H30(0.335582)
 H31(0.349426) H44(0.957178) H39(0.518684) H1A(0.618445) H1B(0.521771)
 H41A(0.54368) H41B(0.639007) H3(0.639444) H2A(0.511408) H2B(0.509466)
 H40A(0.740548) H40B(0.631189) H47(0.999331) H46(1.012761) H49(0.766947)
 H43A(0.806229) H43B(0.90419) H42A(0.79401) H42B(0.761779) H60(0.884134)
 H59(0.801306) H58(0.761379) H61(0.927036) H11(1.246739) H10(1.106638)
 H13(0.973549) H52(0.902107) H51(0.917217) H54(0.833709) H26(0.290858)
 H6(0.93934) H8(0.91032) H5(0.796175) H17(1.423378) H18(1.570029) H19(1.618069)
 H20(1.519459) H25(0.374317) H23(0.654565) H24(0.553947) H56A(0.812168)
 H56B(0.708479) H56C(0.721755) H21A(0.679444) H21B(0.711546) H21C(0.719947)
 H15A(1.287823) H15B(1.177419) H15C(1.251274)
 Fixed Y: H35(0.463738) H36(0.336806) H38(0.435627) H33(0.480997)
 H30(0.754764) H31(0.626636) H44(0.080171) H39(0.195866) H1A(0.384334)
 H1B(0.356157) H41A(0.206408) H41B(0.115482) H3(0.522612) H2A(0.377365)
 H2B(0.478328) H40A(0.081566) H40B(0.080186) H47(-0.094723) H46(-0.059188)
 H49(0.189858) H43A(0.314914) H43B(0.208125) H42A(0.132871) H42B(0.234363) H60(-
 0.19298) H59(-0.018116) H58(0.100356) H61(-0.249373) H11(0.412945)
 H10(0.444457) H13(0.335524) H52(-0.160039) H51(-0.129762) H54(0.168531)
 H26(0.984556) H6(0.53443) H8(0.293116) H5(0.565382) H17(0.188285)
 H18(0.214648) H19(0.31829) H20(0.39557) H25(1.061861) H23(0.88289)
 H24(1.007908) H56A(0.181313) H56B(0.177917) H56C(0.187863) H21A(0.725331)
 H21B(0.784872) H21C(0.673586) H15A(0.170779) H15B(0.253614) H15C(0.162511)
 Fixed Z: H35(0.665875) H36(0.769903) H38(0.645414) H33(0.526172)
 H30(0.511541) H31(0.614738) H44(0.858647) H39(0.85245) H1A(0.999121)
 H1B(1.027301) H41A(0.996134) H41B(1.028004) H3(0.855035) H2A(0.903914)
 H2B(0.917163) H40A(0.905872) H40B(0.916825) H47(0.669238) H46(0.775757)
 H49(0.643676) H43A(0.90873) H43B(0.921755) H42A(0.999297) H42B(1.030855)
 H60(0.15087) H59(0.110632) H58(0.186482) H61(0.26696) H11(0.507716)
 H10(0.614114) H13(0.528192) H52(0.501378) H51(0.60937) H54(0.524411)
 H26(0.27033) H6(0.671445) H8(0.646417) H5(0.775754) H17(0.204842)
 H18(0.131309) H19(0.166756) H20(0.275736) H25(0.163002) H23(0.210527)
 H24(0.133694) H56A(0.311085) H56B(0.369498) H56C(0.281432) H21A(0.404539)
 H21B(0.324242) H21C(0.330329) H15A(0.297949) H15B(0.337568) H15C(0.387497)
;
_shelx_res_checksum              32748
_shelx_hkl_checksum              67584
_shelx_fab_checksum              12676
_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
;