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_1553644
_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_formula_moiety         'C25 H30 F2 Fe N6, 2(B F4), 0.5(C2 H3 N)'
_chemical_formula_sum            'C26 H31.5 B2 F10 Fe N6.5'
_chemical_formula_weight         702.55
_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
_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                110.254(3)
_cell_angle_beta                 106.434(3)
_cell_angle_gamma                91.133(3)
_cell_formula_units_Z            4
_cell_length_a                   11.4603(7)
_cell_length_b                   14.9231(8)
_cell_length_c                   18.6992(11)
_cell_measurement_reflns_used    9010
_cell_measurement_temperature    100
_cell_measurement_theta_max      60.094
_cell_measurement_theta_min      4.420
_cell_volume                     2853.0(3)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.02
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            126647
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.419
_diffrn_reflns_theta_min         1.220
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.7115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0800 before and 0.0481 after correction.
The Ratio of minimum to maximum transmission is 0.9538.
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    1.636
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_recrystallization_method
'Single crystals were grown by vapor diffusion of diethyl ether into a dark yellow acetonitrile solution of the complex'
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.109
_refine_diff_density_max         1.613
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     843
_refine_ls_number_reflns         16997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0409P)^2^+4.5304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14741
_reflns_number_total             16997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04287b2.cif
_cod_data_source_block           aet11_work
_cod_original_formula_sum        'C26 H31.50 B2 F10 Fe N6.50'
_cod_database_code               1553644
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.817
_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
 Sof(F20A)=1-FVAR(1)
 Sof(F20)=FVAR(1)
 Sof(F19A)=1-FVAR(2)
 Sof(F19)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C14(H14A,H14B), C20(H20A,H20B), C26(H26A,H26B), C27(H27A,H27B),
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B),
  C39(H39A,H39B), C45(H45A,H45B)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
 C25(H25), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C48(H48),
  C49(H49), C50(H50)
3.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C38(H38A,H38B,H38C), C52(H52A,H52B,H52C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-05-28
_olex2_date_sample_submission    2016-05-28
_olex2_exptl_crystal_mounting_method 'Mounted in Paratone-N oil'
_olex2_submission_original_sample_id aet11
_olex2_submission_special_instructions 'No special instructions were received'