Ratiometric Quantitation of Redox Status with a Molecular Fe2 Magnetic Resonance Probe
Du, Kang; Waters, Emily Alex; Harris, David David; Chem. Sci.  (2017) –; doi:10.1039/C7SC00562H

data_1545772
_publ_section_title
;
 Ratiometric Quantitation of Redox Status with a Molecular Fe2 Magnetic
 Resonance Probe
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC00562H
_journal_year                    2017
_chemical_formula_moiety         'C19 H29 Fe2 N6 O12 P2, 2(O1), 4(H2 O), H O'
_chemical_formula_sum            'C19 H38 Fe2 N6 O19 P2'
_chemical_formula_weight         828.19
_chemical_properties_physical    ', Air-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-02-05 deposited with the CCDC.
2017-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.3916(7)
_cell_length_b                   9.4099(3)
_cell_length_c                   16.1292(5)
_cell_measurement_reflns_used    9100
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      2.53
_cell_volume                     3246.69(18)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.04
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45560
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.505
_diffrn_reflns_theta_min         2.285
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.081
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0946 before and 0.0485 after correction.
The Ratio of minimum to maximum transmission is 0.8708.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       plate
_exptl_crystal_F_000             1712
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_size_max          0.451
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.14(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.237
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         6605
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.234
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0497
_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^)+19.7952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1170
_reflns_Friedel_coverage         0.929
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                6474
_reflns_number_total             6605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc00562h2.cif
_cod_data_source_block           LFe2Lprime
_cod_database_code               1545772
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.86(3) 0.14(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Rigid bond restraints
 N4, C14, C16
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C18, C19
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O2, N2, N3, C3, C4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O3, C5, C6, C7, C11, C12
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Fe1, P2, O4, O7, C17
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
N4 \\sim C14 \\sim C16: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
C18 \\sim C19: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
O2 \\sim N2 \\sim N3 \\sim C3 \\sim C4: within 2A with sigma of 0.002 and sigma
for terminal atoms of 0.004
O3 \\sim C5 \\sim C6 \\sim C7 \\sim C11 \\sim C12: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004
Fe1 \\sim P2 \\sim O4 \\sim O7 \\sim C17: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
5. Others
 Sof(O20A)=1-FVAR(1)
 Sof(O20)=FVAR(1)
 Sof(O21A)=1-FVAR(2)
 Sof(O21)=FVAR(2)
6.a Free rotating group:
 O14(H14C,H14D), O18(H18A,H18B), O16(H16A,H16B)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2C,H2D), C4(H4A,H4B), C5(H5C,H5D), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B)
6.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10)
6.d X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N5(H5A,H5B), N6(H6A,H6B)
6.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C19(H19A,H19B,H19C)
6.f Idealised tetrahedral OH refined as rotating group:
 O12(H12)
;
_shelx_res_checksum              73542
_shelx_hkl_checksum              18257
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'