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_1553645
_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         '1(C25 H30 F2 N6 Zn), 2(B F4)'
_chemical_formula_sum            'C25 H30 B2 F10 N6 Zn'
_chemical_formula_weight         691.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 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                90
_cell_angle_beta                 90.8750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6092(4)
_cell_length_b                   14.5112(4)
_cell_length_c                   14.1222(4)
_cell_measurement_reflns_used    9672
_cell_measurement_temperature    100
_cell_measurement_theta_max      60.095
_cell_measurement_theta_min      5.611
_cell_volume                     2788.61(14)
_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      99.87
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            80246
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.218
_diffrn_reflns_theta_min         2.495
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0779 before and 0.0543 after correction.
The Ratio of minimum to maximum transmission is 0.9192.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       plate
_exptl_crystal_F_000             1408
_exptl_crystal_recrystallization_method
'Colorless plates were grown by vapor diffusion of diethyl ether into a concentrated light orange solution of the complex in methanol/acetonitrile 2:1'
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.187
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 6399 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     842
_refine_ls_number_reflns         16461
_refine_ls_number_restraints     393
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0492P)^2^+2.5797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1088
_reflns_Friedel_coverage         0.990
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                14525
_reflns_number_total             16461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04287b2.cif
_cod_data_source_block           aet-18_monoclinic
_cod_database_code               1553645
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.775
_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. Restrained distances
 C52-C51
 1.5 with sigma of 0.01
 C38-C37
 1.5 with sigma of 0.01
 C44-C45
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(F23) = Uanis(F24) = Uanis(F22)
4. Rigid body (RIGU) restrains
 Zn2, N7, N8, N9, N10, N11, N12, C26, C31, C32, C27, C28, C39, C29, C30, C46,
 C47, C51, C33, C37, C40, C44, H26a, H26b, H31a, H31b, H32a, H32b, H27a, H27b,
 H28a, H28b, H39a, H39b, H29a, H29b, H30a, H30b, H46a, H46b, C48, C50, C52, C34,
  C36, C38, C41, C43, C45, C49, F4, F3, C35, H36, F5, C42, H49, H35, H41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(F3)+Sof(H34)+Sof(H37)+Sof(C38)+Sof(H38a)+Sof(H38b)+Sof(H38c)]+1*
 [Sof(F5)+Sof(H41)+Sof(H44)+Sof(C45)+Sof(H45a)+Sof(H45b)+Sof(H45c)]+1*[Sof(H48)+
 Sof(H51)+Sof(C52)+Sof(H52a)+Sof(H52b)+Sof(H52c)+Sof(F4)]=2 with esd of 0.001
 Sof(F22)=Sof(F23)=Sof(F24)=1-FVAR(1)
 Sof(F18)=Sof(F19)=Sof(F20)=FVAR(1)
 Sof(H34)=Sof(C38)=Sof(H38a)=Sof(H38b)=Sof(H38c)=1-FVAR(2)
 Sof(F3)=Sof(H37)=FVAR(2)
 Sof(H41)=Sof(C45)=Sof(H45a)=Sof(H45b)=Sof(H45c)=1-FVAR(3)
 Sof(F5)=Sof(H44)=FVAR(3)
 Sof(H48)=Sof(C52)=Sof(H52a)=Sof(H52b)=Sof(H52c)=1-FVAR(4)
 Sof(H51)=Sof(F4)=FVAR(4)
6.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), C46(H46a,H46b)
6.b Me refined with riding coordinates:
 C52(H52a,H52b,H52c)
6.c 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), C41(H41), C42(H42), C43(H43), C44(H44), C34(H34), C35(H35), C36(H36),
  C37(H37), C48(H48), C49(H49), C50(H50), C51(H51)
6.d Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C45(H45a,H45b,H45c), C38(H38a,H38b,H38c)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_completion    2016-07-25
_olex2_date_sample_data_collection 2016-07-24
_olex2_date_sample_submission    2016-07-24
_olex2_exptl_crystal_mounting_method 'Crystal was mounted in Paratone-N oil'
_olex2_submission_original_sample_id aet18
_olex2_submission_special_instructions 'No special instructions were received'