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_1549508
_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         'C29 H21 Co N7 O5, 2(C4 H12 N), C2 H3 N'
_chemical_formula_sum            'C39 H48 Co N10 O5'
_chemical_formula_weight         795.80
_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             2017-07-06
_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                105.524(2)
_cell_angle_beta                 98.363(2)
_cell_angle_gamma                94.721(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2617(2)
_cell_length_b                   11.3806(2)
_cell_length_c                   19.5188(4)
_cell_measurement_reflns_used    22178
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      31.0140
_cell_measurement_theta_min      2.1090
_cell_volume                     2155.33(8)
_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 0.999
_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    -69.00  -7.00   0.50    9.50    --    3.71 -37.00 120.00  124
  2  \w    -26.00  36.00   0.50    9.50    --    3.71 -99.00  60.00  124
  3  \w    -21.00   9.00   0.50    9.50    --   -4.80 -99.00 120.00   60
  4  \w     -7.00  74.00   0.50    9.50    --    3.71  37.00   0.00  162
  5  \w    -10.00  76.00   0.50    9.50    --    3.71  57.00-120.00  172
  6  \w    -23.00   2.00   0.50    9.50    --   -4.80  77.00  60.00   50
  7  \w    -26.00  36.00   0.50    9.50    --    3.71 -99.00-115.00  124
  8  \w    -26.00  24.00   0.50    9.50    --   -4.80 -99.00-115.00  100
  9  \w    -26.00  35.00   0.50    9.50    --    3.71 -99.00-150.00  122
;
_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      0.0275711000
_diffrn_orient_matrix_UB_12      -0.0428952000
_diffrn_orient_matrix_UB_13      0.0165395000
_diffrn_orient_matrix_UB_21      -0.0235242000
_diffrn_orient_matrix_UB_22      -0.0479714000
_diffrn_orient_matrix_UB_23      -0.0322720000
_diffrn_orient_matrix_UB_31      0.0603960000
_diffrn_orient_matrix_UB_32      0.0105690000
_diffrn_orient_matrix_UB_33      -0.0123300000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36570
_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         1.872
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.685
_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 purple'
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       block
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8798
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0409P)^2^+0.7048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7941
_reflns_number_total             8798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01621f2.cif
_cod_data_source_block           rlacy3_abs
_cod_depositor_comments
'Adding full bibliography for 1549501--1549509.cif.'
_cod_database_code               1549508
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C39H48CoN10O5
_chemical_oxdiff_usercomment
'Crystallized from DMA, acetonitrile and diethyl ether'
_reflns_odcompleteness_completeness 98.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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. Uiso/Uaniso restraints and constraints
N10 \\sim C38 \\sim C39: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
3. Rigid body (RIGU) restrains
 N10, C38, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C19(H19A,H19B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C13(H13), C14(H14), C16(H16), C17(H17),
 C22(H22), C23(H23), C25(H25), C26(H26)
4.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              63099
_shelx_fab_checksum              24604
_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 1.083
_oxdiff_exptl_absorpt_empirical_full_min 0.923