Deciphering the mechanism of O<sub>2</sub> reduction with electronically tunable non-heme iron enzyme model complexes.
Surendhran, Roshaan; D'Arpino, Alexander A; Sciscent, Bao Y.; Cannella, Anthony F.; Friedman, Alan E.; MacMillan, Samantha N.; Gupta, Rupal; Lacy, David C.; Chemical science 9 (2018) 5773–5780; doi:10.1039/c8sc01621f

data_1549502
_publ_section_title
;
 Deciphering the mechanism of O<sub>2</sub> reduction with electronically
 tunable non-heme iron enzyme model complexes.
;
_journal_issue                   26
_journal_name_full               'Chemical science'
_journal_page_first              5773
_journal_page_last               5780
_journal_paper_doi               10.1039/c8sc01621f
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C48 H36 Fe2 N14 O19, 2(C4 H12 N)'
_chemical_formula_sum            'C56 H60 Fe2 N16 O19'
_chemical_formula_weight         1372.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-21
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2016.08.26 svn.r3337 for Rigaku Oxford Diffraction, GUI svn.r5221)
;
_audit_update_record
;
2018-03-28 deposited with the CCDC.
2018-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                68.492(4)
_cell_angle_beta                 83.722(4)
_cell_angle_gamma                66.929(4)
_cell_formula_units_Z            1
_cell_length_a                   11.3590(5)
_cell_length_b                   11.8525(5)
_cell_length_c                   13.7993(6)
_cell_measurement_reflns_used    12607
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.0080
_cell_measurement_theta_min      3.4120
_cell_volume                     1588.95(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -12.00  78.00   0.50    3.00    --   47.80 -95.00  24.00  180
  2  \w     36.00  85.50   0.50   12.00    --  107.75 -95.00  24.00   99
  3  \w     51.00  99.00   0.50   12.00    --  107.75 -94.00 -60.00   96
  4  \w     77.00 120.00   0.50   12.00    --  107.75-125.00-120.00   86
  5  \w     90.00 120.00   0.50   12.00    --  107.75-125.00-180.00   60
  6  \w     78.00 103.00   0.50   12.00    --  107.75 -94.00-150.00   50
  7  \w     59.00 122.00   0.50   12.00    --  107.75 -61.00-120.00  126
  8  \w     73.00 100.00   0.50   12.00    --  107.75 -45.00-120.00   54
  9  \w     44.00 100.50   0.50   12.00    --  107.75 -45.00 -60.00  113
 10  \w    126.00 169.00   0.50   12.00    --  107.75  30.00-150.00   86
 11  \w    120.00 144.00   0.50   12.00    --  107.75  61.00 -60.00   48
 12  \w    148.00 176.00   0.50   12.00    --  107.75 125.00 -60.00   56
 13  \w    142.00 174.00   0.50   12.00    --  107.75  61.00  60.00   64
 14  \w    105.00 135.00   0.50   12.00    --  107.75  61.00  60.00   60
 15  \w    102.00 178.00   0.50   12.00    --  107.75  95.00 134.00  152
 16  \w     85.00 178.00   0.50   12.00    --  107.75  79.00  72.19  186
 17  \w     93.00 118.00   0.50   12.00    --  107.75 125.00 -60.00   50
 18  \w     34.00 118.00   0.50   12.00    --  107.75 -15.00 150.00  168
 19  \w     59.00  93.00   0.50   12.00    --  107.75 -45.00  30.00   68
 20  \w     36.00  77.50   0.50   12.00    --  107.75 -77.00 120.00   83
 21  \w     35.00 119.00   0.50   12.00    --  107.75 -30.00 -30.00  168
 22  \w     36.00  79.00   0.50   12.00    --  107.75-125.00   0.00   86
 23  \w     38.00 119.00   0.50   12.00    --  107.75 -30.00 150.00  162
 24  \w     36.00 119.00   0.50   12.00    --  107.75 -45.00 150.00  166
 25  \w     36.00  79.50   0.50   12.00    --  107.75-125.00  90.00   87
 26  \w     36.00 130.00   0.50   12.00    --  107.75 -77.00 -30.00  188
 27  \w     36.00 106.00   0.50   12.00    --  107.75 -94.00-120.00  140
 28  \w     44.00  85.00   0.50   12.00    --  107.75-125.00-180.00   82
 29  \w     -4.00  80.00   0.50    3.00    --   47.80 -99.00-120.00  168
 30  \w     34.00 118.00   0.50   12.00    --  107.75 -15.00  60.00  168
 31  \w     36.00 119.00   0.50   12.00    --  107.75-125.00 150.00  166
 32  \w    -58.00  27.00   0.50    3.00    --  -47.80  19.00  90.00  170
 33  \w    -58.00  25.00   0.50    3.00    --  -47.80  37.00  60.00  166
 34  \w    -78.00  24.00   0.50    3.00    --  -47.80  95.00 134.00  204
 35  \w    -82.00 -14.00   0.50   12.00    --  -86.25  95.00 134.00  136
 36  \w   -119.00 -26.00   0.50    3.00    --  -47.80 -77.00 120.00  186
 37  \w   -119.00 -70.00   0.50    3.00    --  -47.80-125.00   0.00   98
 38  \w   -119.00 -70.00   0.50    3.00    --  -47.80-125.00-180.00   98
 39  \w   -158.00 -80.00   0.50   12.00    --  -86.25 -95.00  24.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1279140000
_diffrn_orient_matrix_UB_12      0.1189785000
_diffrn_orient_matrix_UB_13      -0.0196133000
_diffrn_orient_matrix_UB_21      -0.0123382000
_diffrn_orient_matrix_UB_22      0.0003044000
_diffrn_orient_matrix_UB_23      -0.1101764000
_diffrn_orient_matrix_UB_31      -0.0724695000
_diffrn_orient_matrix_UB_32      -0.0930787000
_diffrn_orient_matrix_UB_33      0.0435747000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25342
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.057
_diffrn_reflns_theta_min         3.445
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.381
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0504
_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^)+(0.1050P)^2^+0.6431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5623
_reflns_number_total             6012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01621f2.cif
_cod_data_source_block           rlacy2_abs
_cod_depositor_comments
'Adding full bibliography for 1549501--1549509.cif.'
_cod_original_cell_volume        1588.95(13)
_cod_database_code               1549502
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C62H62Fe2N10O19
_chemical_oxdiff_usercomment
'Crystallized from acetonitrileand diethyl ether'
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C12(H12), C13(H13), C15(H15), C16(H16),
 C20(H20), C21(H21), C23(H23), C24(H24)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C)
;
_shelx_res_checksum              710
_shelx_fab_checksum              59998
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.113
_oxdiff_exptl_absorpt_empirical_full_min 0.682