Crystal structure of gluconate bound iron(iii) complex: synthesis, characterization and redox properties of the complex in aqueous solution
Stewart, Christopher D.; Arman, Hadi; Benavides, Brenda; Musie, Ghezai T.; New Journal of Chemistry 42 (2018) 15088–; doi:10.1039/C8NJ01886C

data_7057587
_publ_section_title
;
 Crystal structure of gluconate bound iron(iii) complex: synthesis,
 characterization and redox properties of the complex in aqueous solution
;
_journal_issue                   18
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15088
_journal_paper_doi               10.1039/C8NJ01886C
_journal_volume                  42
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         '0.5(C232 H240 Fe16 K22 N24 O171.6), 1.8(O)'
_chemical_formula_sum            'C116 H120 Fe8 K11 N12 O87.6'
_chemical_formula_weight         3960.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-11-10 deposited with the CCDC.
2018-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.4006(8)
_cell_length_b                   19.7985(7)
_cell_length_c                   22.1693(15)
_cell_measurement_reflns_used    21051
_cell_measurement_temperature    98
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.1
_cell_volume                     8515.3(7)
_computing_cell_refinement
;
CrystalClear-SM Auto 2.0 r5 (Rigaku, 2010)
;
_computing_data_collection
;
CrystalClear-SM Auto 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
CrystalClear-SM Auto 2.0 r5 (Rigaku, 2010)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      98
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
scan:
    Number of images: 216
               Slice: -68.0000 - 40.0000
         Image width: 0.5000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 70.0000
                 Phi: 0.0000
                 XTD: 35.0000
              2theta: -35.0000
scan:
    Number of images: 66
               Slice: 2.0000 - 35.0000
         Image width: 0.5000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 70.0000
                 Phi: 270.0000
                 XTD: 35.0000
              2theta: -35.0000
;
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724 (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.050766
_diffrn_orient_matrix_UB_12      -0.008746
_diffrn_orient_matrix_UB_13      0.000119
_diffrn_orient_matrix_UB_21      -0.000629
_diffrn_orient_matrix_UB_22      -0.004270
_diffrn_orient_matrix_UB_23      -0.044943
_diffrn_orient_matrix_UB_31      0.008904
_diffrn_orient_matrix_UB_32      0.049562
_diffrn_orient_matrix_UB_33      -0.003851
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14736
_diffrn_reflns_point_group_measured_fraction_full 0.931
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         3.080
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.033
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            'clear yellowish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       needle
_exptl_crystal_F_000             4036
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.284
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Flack x determined using 4786 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1105
_refine_ls_number_reflns         14736
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1661
_reflns_Friedel_coverage         0.725
_reflns_Friedel_fraction_full    0.859
_reflns_Friedel_fraction_max     0.857
_reflns_number_gt                12970
_reflns_number_total             14736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj01886c2.cif
_cod_data_source_block           cd1012a
_cod_depositor_comments          'Adding full bibliography for 7057587.cif.'
_cod_original_formula_sum        'C116 H120 Fe8 K11 N12 O87.60'
_cod_database_code               7057587
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H20-O20
 0.85 with sigma of 0.02
 H57-C57
 0.95 with sigma of 0.02
 H20-O19
 1.6 with sigma of 0.01
 H26-O26
 0.84 with sigma of 0.01
 O32_$1-H26
 2.1 with sigma of 0.01
 O25-H25
 1 with sigma of 0.01
 H25-O13
 1.9 with sigma of 0.01
 H31-O31
 1.05 with sigma of 0.01
 H31-O48
 2.1 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O27) = Uanis(C52) = Uanis(C51) = Uanis(C50)
4. Others
 Fixed Sof: N6(0.5) O39(0.5) K5A(0.5) O45A(0.5) K5B(0.5) O46B(0.5) O42(0.5)
 O43(0.5) O44(0.5) K6(0.5) O48(0.4) O47(0.5) O49(0.4) O50(0.5) O52(0.5) N7(0.5)
 O51(0.5)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C35(H35), C54(H54), C49(H49), C56(H56), C55(H55), C50(H50), C51(H51)
5.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C8(H8A,H8B), C39(H39A,H39B), C36(H36A,H36B), C16(H16A,H16B),
 C37(H37A,H37B), C11(H11A,H11B), C13(H13A,H13B), C34(H34A,H34B), C32(H32A,H32B),
  C58(H58A,H58B), C14(H14A,H14B), C52(H52A,H52B)
5.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C41(H41), C18(H18), C25(H25A), C26(H26A), C21(H21), C44(H44),
 C20(H20A), C5(H5), C19(H19), C2(H2), C4(H4), C3(H3), C42(H42), C43(H43),
 C27(H27)
5.d Tetrahedral OH refined with riding coordinates:
 O34(H34), O30(H30), O32(H32), O27(H27A)
;
_shelx_res_checksum              52122
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'glass fiber'
_olex2_submission_special_instructions 'No special instructions were received'