Spin-crossover and high-spin iron(ii) complexes as chemical shift <sup>19</sup>F magnetic resonance thermometers.
Thorarinsdottir, Agnes E.; Gaudette, Alexandra I.; Harris, T. David; Chemical science 8 (2017) 2448–2456; doi:10.1039/c6sc04287b

data_1553646
_publ_section_title
;
 Spin-crossover and high-spin iron(ii) complexes as chemical shift
 <sup>19</sup>F magnetic resonance thermometers.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              2448
_journal_page_last               2456
_journal_paper_doi               10.1039/c6sc04287b
_journal_volume                  8
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         '3(C8 H9 F Fe0.33 N2), 2(B F4)'
_chemical_formula_sum            'C24 H27 B2 F11 Fe N6'
_chemical_formula_weight         685.98
_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_Hall           'P 3'
_space_group_name_H-M_alt        'P 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-20 deposited with the CCDC.
2017-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   16.8376(5)
_cell_length_b                   16.8376(5)
_cell_length_c                   7.8829(3)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.662
_cell_measurement_theta_min      9.834
_cell_volume                     1935.43(11)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.08
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            115769
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         36.445
_diffrn_reflns_theta_min         4.843
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.7068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0857 before and 0.0536 after correction.
The Ratio of minimum to maximum transmission is 0.9461.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       prism
_exptl_crystal_F_000             1044
_exptl_crystal_recrystallization_method
'Crystals were grown by vapor diffusion of diethyl ether into a concentrated red-colored solution of the complex in methanol/acetonitrile (1:1) mixture'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.309
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 6029 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.077(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         12595
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0632P)^2^+0.5295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.0958
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                12363
_reflns_number_total             12595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04287b2.cif
_cod_data_source_block           aet15_work
_cod_original_cell_volume        1935.43(14)
_cod_database_code               1553646
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.808
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5055(12) 0.4945(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Others
 Sof(F10A)=1-FVAR(1)
 Sof(F10)=FVAR(1)
 Sof(F11A)=1-FVAR(2)
 Sof(F11)=FVAR(2)
 Sof(F9A)=1-FVAR(3)
 Sof(F9)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C17(H17a,H17b), C18(H18a,H18b),
 C19(H19a,H19b), C9(H9a,H9b), C10(H10a,H10b), C11(H11a,H11b)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C22(H22), C23(H23), C24(H24), C14(H14), C15(H15),
 C16(H16)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-07-09
_olex2_date_sample_submission    2016-07-09
_olex2_exptl_crystal_mounting_method 'Crystal was mounted in Paratone-N oil'
_olex2_submission_original_sample_id aet15
_olex2_submission_special_instructions 'No special instructions were received'