Effect of Chelation on Iron‒Chromium Redox Flow Batteries
Waters, Scott E.; Robb, Brian H.; Marshak, Michael P.; ACS Energy Letters  (2020) 1758–1762; doi:10.1021/acsenergylett.0c00761

data_4517651
_publ_section_title
;
 Effect of Chelation on Iron--Chromium Redox Flow Batteries
;
_journal_name_full               'ACS Energy Letters'
_journal_page_first              1758
_journal_page_last               1762
_journal_paper_doi               10.1021/acsenergylett.0c00761
_journal_year                    2020
_chemical_formula_moiety         'C14 H22 Fe K2 N3 O12, H2 O'
_chemical_formula_sum            'C14 H24 Fe K2 N3 O13'
_chemical_formula_weight         576.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.386(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1983(15)
_cell_length_b                   6.9475(7)
_cell_length_c                   18.7656(17)
_cell_measurement_reflns_used    9168
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.640
_cell_measurement_theta_min      2.670
_cell_volume                     2105.7(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      110.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0372
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            71268
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.654
_diffrn_reflns_theta_min         2.177
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.187
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1029 before and 0.0603 after correction. The Ratio of minimum to maximum transmission is 0.8737. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_description       prism
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.528
_exptl_crystal_size_mid          0.329
_exptl_crystal_size_min          0.238
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         6465
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0216P)^2^+3.5978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5927
_reflns_number_total             6465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nz0c00761_si_002.cif
_cod_data_source_block           K2FeDTPA
_cod_depositor_comments          'Adding full bibliography for 4517651.cif.'
_cod_database_code               4517651
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.765
_shelx_estimated_absorpt_t_min   0.573
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O11-H11B = O11-H11A = O12_$1-H12B_$1 = O12_$1-H12A_$1
 0.87 with sigma of 0.02
 O13-H13D = O13-H13C
 0.87 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11C,
 H11D), C12(H12C,H12D), C13(H13A,H13B), C14(H14A,H14B)
;
_olex2_submission_special_instructions 'No special instructions were received'