Cobalt Superoxo and Alkylperoxo Complexes Derived from Reaction of Ring-Cleaving Dioxygenase Models with O<sub>2</sub>.
Kumar, Praveen; Lindeman, Sergey V.; Fiedler, Adam T.; Journal of the American Chemical Society 141 (2019) 10984–10987; doi:10.1021/jacs.9b05320

data_4127418
_publ_section_title
;
 Cobalt Superoxo and Alkylperoxo Complexes Derived from Reaction of
 Ring-Cleaving Dioxygenase Models with O<sub>2</sub>.
;
_journal_issue                   28
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10984
_journal_page_last               10987
_journal_paper_doi               10.1021/jacs.9b05320
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C29 H42 B Co N6 O2, C2 H3 N'
_chemical_formula_sum            'C31 H45 B Co N7 O2'
_chemical_formula_weight         617.48
_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     iterative
_audit_creation_date             2018-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                84.589(2)
_cell_angle_beta                 87.358(2)
_cell_angle_gamma                68.153(3)
_cell_formula_units_Z            2
_cell_length_a                   7.7385(2)
_cell_length_b                   10.0689(3)
_cell_length_c                   22.2625(6)
_cell_measurement_reflns_used    15797
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.5650
_cell_measurement_theta_min      3.9680
_cell_volume                     1602.78(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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    -67.00  32.00   1.00    2.00    --  -42.33  37.00 -30.00   99
  2  \w   -122.00  -1.00   1.00    2.00    --  -42.33 -19.00 150.00  121
  3  \w     23.00  98.00   1.00    2.00    --   42.33-125.00  60.00   75
  4  \w     23.00  98.00   1.00    2.00    --   42.33-125.00 120.00   75
  5  \w     27.00 126.00   1.00    8.00    --  100.00 -45.00-180.00   99
  6  \w     74.00 173.00   1.00    8.00    --  100.00  45.00 150.00   99
  7  \w     17.00 109.00   1.00    8.00    --  100.00 -94.00-180.00   92
  8  \w     17.00 109.00   1.00    8.00    --  100.00 -94.00 -90.00   92
  9  \w     71.00 172.00   1.00    8.00    --  100.00  61.00 -30.00  101
 10  \w     28.00 129.00   1.00    8.00    --  100.00 -61.00  30.00  101
 11  \w     17.00 109.00   1.00    8.00    --  100.00 -94.00  60.00   92
 12  \w     17.00 109.00   1.00    8.00    --  100.00 -94.00   0.00   92
 13  \w     18.00 153.00   1.00    8.00    --  100.00 -15.00 -30.00  135
 14  \w     67.00 176.00   1.00    8.00    --  100.00  77.00  30.00  109
 15  \w     27.00 121.00   1.00    8.00    --  100.00-125.00   0.00   94
 16  \w     74.00 173.00   1.00    8.00    --  100.00  45.00-120.00   99
 17  \w   -114.00 -14.00   1.00    2.00    --  -42.33 -57.00  60.00  100
 18  \w   -118.00 -10.00   1.00    2.00    --  -42.33 -77.00  30.00  108
 19  \w   -118.00 -10.00   1.00    2.00    --  -42.33 -77.00 -30.00  108
 20  \w   -118.00 -10.00   1.00    2.00    --  -42.33 -77.00-150.00  108
 21  \w     67.00 113.00   1.00    8.00    --  100.00  77.00  90.00   46
 22  \w     71.00 172.00   1.00    8.00    --  100.00  61.00-180.00  101
 23  \w     67.00 176.00   1.00    8.00    --  100.00  77.00 -90.00  109
 24  \w     71.00 172.00   1.00    8.00    --  100.00  61.00 150.00  101
 25  \w     71.00 172.00   1.00    8.00    --  100.00  61.00  90.00  101
 26  \w     67.00 176.00   1.00    8.00    --  100.00  77.00-180.00  109
 27  \w     67.00 176.00   1.00    8.00    --  100.00  77.00-120.00  109
 28  \w     71.00 172.00   1.00    8.00    --  100.00  61.00   0.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0054815000
_diffrn_orient_matrix_UB_12      0.0561855000
_diffrn_orient_matrix_UB_13      -0.0669662000
_diffrn_orient_matrix_UB_21      -0.0084407000
_diffrn_orient_matrix_UB_22      -0.1411824000
_diffrn_orient_matrix_UB_23      -0.0183614000
_diffrn_orient_matrix_UB_31      -0.2142608000
_diffrn_orient_matrix_UB_32      0.0653673000
_diffrn_orient_matrix_UB_33      0.0032656000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29722
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        70.620
_diffrn_reflns_theta_max         70.620
_diffrn_reflns_theta_min         3.989
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.502
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.308
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (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            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       needle
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.00047(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0349P)^2^+0.6171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5893
_reflns_number_total             6091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05320_si_002.cif
_cod_data_source_block           Complex4
_cod_database_code               4127418
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C29 H43 B N6 O2 Co C2 H3 N'
_shelx_estimated_absorpt_t_max   0.858
_shelx_estimated_absorpt_t_min   0.173
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C8(H8), C18(H18), C20(H20)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C),
 C29(H29A,H29B,H29C), C31(H31A,H31B,H31C)
;
_olex2_date_sample_data_collection 2018-03-17
_olex2_date_sample_submission    2018-03-15
_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 1.111
_oxdiff_exptl_absorpt_empirical_full_min 0.854