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_1549501
_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
'C50 H39 Fe2 N14 O21, 3(C4 H12 N), 2(C4 H10 O)'
_chemical_formula_sum            'C70 H95 Fe2 N17 O23'
_chemical_formula_weight         1654.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-22
_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                90
_cell_angle_beta                 95.002(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2471(3)
_cell_length_b                   18.3327(5)
_cell_length_c                   17.6262(5)
_cell_measurement_reflns_used    14304
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.7860
_cell_measurement_theta_min      1.9870
_cell_volume                     3942.41(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -28.00  57.00   0.50   10.50    --   -6.42  79.00  -0.00  170
  2  \w    -69.00  15.00   0.50   10.50    --   -6.42 -79.00-124.00  168
  3  \w     -4.00  26.00   0.50   10.50    --   -6.42 -99.00 -90.00   60
  4  \w    -23.00  15.00   0.50   10.50    --   -6.42 -99.00  60.00   76
  5  \w    -24.00  18.00   0.50   10.50    --   -6.42 -99.00 120.00   84
  6  \w    -17.00   8.00   0.50   10.50    --   -6.42 -99.00  90.00   50
;
_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      -0.0532209000
_diffrn_orient_matrix_UB_12      -0.0154735000
_diffrn_orient_matrix_UB_13      -0.0051458000
_diffrn_orient_matrix_UB_21      -0.0208263000
_diffrn_orient_matrix_UB_22      0.0291410000
_diffrn_orient_matrix_UB_23      0.0209113000
_diffrn_orient_matrix_UB_31      -0.0107356000
_diffrn_orient_matrix_UB_32      0.0201987000
_diffrn_orient_matrix_UB_33      -0.0341711000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37576
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.005
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
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 brown'
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       block
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.134
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         8075
_refine_ls_number_restraints     260
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0987P)^2^+3.9722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1660
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6595
_reflns_number_total             8075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01621f2.cif
_cod_data_source_block           rlacy10_abs
_cod_depositor_comments
'Adding full bibliography for 1549501--1549509.cif.'
_cod_database_code               1549501
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C70H97Fe2N17O23
_chemical_oxdiff_usercomment     'Crystallized from DMA/ether.'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.67
_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. Restrained distances
 N1A-C1 \\sim N1B-C1 \\sim N5B-C14 \\sim N5A-C14
 with sigma of 0.02
 O1A-N1A \\sim O1B-N1B \\sim O2A-N1A \\sim O2B-N1B \\sim O5B-N5B \\sim O5A-N5A
\\sim O6A-N5A \\sim O6B-N5B
 with sigma of 0.02
 N9-C32A \\sim N9-C32B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1A \\sim O2A \\sim N1A \\sim O1B \\sim O2B \\sim N1B \\sim O5B \\sim O6B \\sim
N5B \\sim O5A \\sim N5A \\sim O6A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O12 \\sim C33 \\sim C34 \\sim C35 \\sim C36: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O1A, O2A, N1A, O1B, O2B, N1B, O5B, O6B, N5B, O5A, N5A, O6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O12, C33, C34, C35, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O1B)=Sof(O2B)=Sof(N1B)=1-FVAR(1)
 Sof(O1A)=Sof(O2A)=Sof(N1A)=FVAR(1)
 Sof(C32B)=Sof(H32A)=Sof(H32B)=Sof(H32C)=1-FVAR(2)
 Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=FVAR(2)
 Sof(O5B)=Sof(O6B)=Sof(N5B)=1-FVAR(3)
 Sof(O5A)=Sof(N5A)=Sof(O6A)=FVAR(3)
 Fixed Sof: H26A(0.5) H26B(0.5) H26C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C17(H17A,H17B), C34(H34A,H34B), C35(H35A,H35B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C15(H15), C16(H16),
 C20(H20), C21(H21), C23(H23), C24(H24)
6.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C31(H31A,
 H31B,H31C), C32B(H32A,H32B,H32C), C32A(H32D,H32E,H32F)
;
_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 1.274
_oxdiff_exptl_absorpt_empirical_full_min 0.862