pH-Dependent Spin State Population and 19F NMR Chemical Shift via Remote Ligand Protonation in an Iron(II) Complex
Gaudette, Alexandra; Thorarinsdottir, Agnes E.; Harris, David; Chemical Communications  (2017) –; doi:10.1039/C7CC08158H

data_7120865
_publ_section_title
;
 pH-Dependent Spin State Population and 19F NMR Chemical Shift via Remote
 Ligand Protonation in an Iron(II) Complex
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C7CC08158H
_journal_year                    2017
_chemical_formula_moiety         'C29 H39 F Fe N6 O2, 2(B F4)'
_chemical_formula_sum            'C29 H39 B2 F9 Fe N6 O2'
_chemical_formula_weight         752.13
_chemical_properties_physical    Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-09-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-09-12 deposited with the CCDC.
2017-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.049(11)
_cell_length_b                   14.809(10)
_cell_length_c                   29.11(2)
_cell_measurement_reflns_used    6047
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.009
_cell_measurement_theta_min      2.384
_cell_volume                     6487(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            51003
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.422
_diffrn_reflns_theta_min         1.947
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0692 before and 0.0430 after correction. The Ratio of minimum to maximum transmission is 0.9348. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear orangish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       block
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.076
_refine_diff_density_max         1.361
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         5963
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.0785
_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^)+(0.0867P)^2^+32.7299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1898
_refine_ls_wR_factor_ref         0.2152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3938
_reflns_number_total             5963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc08158h2.cif
_cod_data_source_block           aig91ortho
_cod_original_cell_volume        6486(8)
_cod_database_code               7120865
_shelx_shelxl_version_number     2014/7
_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. Uiso/Uaniso restraints and constraints
Uanis(F7A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Others
 Sof(F6A)=1-FVAR(1)
 Sof(F6)=FVAR(1)
 Sof(F7A)=1-FVAR(2)
 Sof(F7)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C22(H22a,H22b), C13(H13a,H13b), C11(H11a,H11b), C10(H10a,
 H10b), C9(H9a,H9b), C7(H7a,H7b), C12(H12a,H12b), C8(H8a,H8b)
4.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C29(H29), C3(H3), C4(H4)
4.c Idealised Me refined as rotating group:
 C20(H20a,H20b,H20c), C21(H21a,H21b,H21c), C25(H25a,H25b,H25c), C28(H28a,H28b,
 H28c), C1(H1a,H1b,H1c)
;
_olex2_submission_original_sample_id aig91
_olex2_submission_special_instructions 'No special instructions were received'