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_1553643
_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         'C27 H33 F3 Fe1 N6, 2(B1 F4)'
_chemical_formula_sum            'C27 H33 B2 F11 Fe N6'
_chemical_formula_weight         728.06
_space_group_crystal_system      cubic
_space_group_IT_number           219
_space_group_name_Hall           'F -4a 2 3'
_space_group_name_H-M_alt        'F -4 3 c'
_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
;
2016-09-22 deposited with the CCDC.
2017-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   29.3374(7)
_cell_length_b                   29.3374(7)
_cell_length_c                   29.3374(7)
_cell_measurement_reflns_used    9591
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.103
_cell_measurement_theta_min      5.551
_cell_volume                     25250.2(10)
_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      100.05
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            448528
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         36.356
_diffrn_reflns_theta_min         2.777
_diffrn_source                   'sealed tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1702 before and 0.0673 after correction.
The Ratio of minimum to maximum transmission is 0.8811.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       plate
_exptl_crystal_F_000             11904
_exptl_crystal_preparation
'Single crystals, light yellow plates, were grown by vapor diffusion of diethyl ether into a concentrated dark orange methanol/acetonitrile (1:1) solution of the complex.'
_exptl_crystal_recrystallization_method 'See preparation details'
_exptl_crystal_size_max          0.857
_exptl_crystal_size_mid          0.477
_exptl_crystal_size_min          0.174
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 2050 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         5143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0486
_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^)+(0.1044P)^2^+28.6904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1548
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4500
_reflns_number_total             5143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04287b3.cif
_cod_data_source_block           aet13_trial_cubic
_cod_original_cell_volume        25250.2(18)
_cod_original_sg_symbol_Hall     'F -4c 2 3'
_cod_database_code               1553643
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.640
_olex2_refinement_description
;
1. 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
2. Others
 Fixed Sof: F3(0.33333)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_completion    2016-06-14
_olex2_date_sample_data_collection 2016-06-13
_olex2_date_sample_submission    2016-06-13
_olex2_exptl_crystal_mounting_method 'Crystals were mounted in Paratone-N oil'
_olex2_submission_original_sample_id '[Fe(L2)][BF4]2'
_olex2_submission_special_instructions 'No special instructions were received'