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_4127417
_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 H43 B Co N7 O3, 2(C2 H3 N)'
_chemical_formula_sum            'C33 H49 B Co N9 O3'
_chemical_formula_weight         689.55
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-03-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                87.688(2)
_cell_angle_beta                 87.320(2)
_cell_angle_gamma                66.582(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6841(3)
_cell_length_b                   9.7745(3)
_cell_length_c                   20.6176(6)
_cell_measurement_reflns_used    14175
_cell_measurement_temperature    100.05(10)
_cell_measurement_theta_max      70.5480
_cell_measurement_theta_min      4.9010
_cell_volume                     1788.39(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_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    -71.00  31.00   1.00    4.00    --  -42.46  57.00 -30.00  102
  2  \w   -115.00 -14.00   1.00    4.00    --  -42.46 -57.00-180.00  101
  3  \w      1.00  83.00   1.00    4.00    --   42.46 -99.00  60.00   82
  4  \w     18.00 117.00   1.00    4.00    --   42.46  37.00  90.00   99
  5  \w     71.00 172.00   1.00   16.00    --  100.00  61.00  60.00  101
  6  \w     17.00 110.00   1.00   16.00    --  100.00 -94.00-180.00   93
  7  \w     72.00 176.00   1.00   16.00    --  100.00  30.00-150.00  104
  8  \w     17.00 110.00   1.00   16.00    --  100.00 -94.00  90.00   93
  9  \w     67.00 176.00   1.00   16.00    --  100.00  77.00   0.00  109
 10  \w     28.00 129.00   1.00   16.00    --  100.00 -61.00 120.00  101
 11  \w     74.00 173.00   1.00   16.00    --  100.00  45.00 120.00   99
 12  \w     27.00 118.00   1.00   16.00    --  100.00-125.00  30.00   91
 13  \w     27.00 118.00   1.00   16.00    --  100.00-125.00   0.00   91
 14  \w     94.00 173.00   1.00   16.00    --  100.00 125.00  30.00   79
 15  \w     24.00 128.00   1.00   16.00    --  100.00 -30.00-180.00  104
 16  \w     24.00 133.00   1.00   16.00    --  100.00 -77.00   0.00  109
 17  \w   -115.00 -14.00   1.00    4.00    --  -42.46 -57.00 -60.00  101
 18  \w   -119.00 -10.00   1.00    4.00    --  -42.46 -77.00 -90.00  109
 19  \w   -119.00 -10.00   1.00    4.00    --  -42.46 -77.00-180.00  109
 20  \w   -119.00 -10.00   1.00    4.00    --  -42.46 -77.00  90.00  109
 21  \w    -32.00  67.00   1.00    4.00    --   42.46 -37.00 120.00   99
 22  \w     71.00 172.00   1.00   16.00    --  100.00  61.00 -30.00  101
 23  \w     67.00 150.00   1.00   16.00    --  100.00  77.00 120.00   83
 24  \w     72.00 176.00   1.00   16.00    --  100.00  30.00 -60.00  104
 25  \w     67.00 176.00   1.00   16.00    --  100.00  77.00-180.00  109
 26  \w     67.00 176.00   1.00   16.00    --  100.00  77.00 -90.00  109
 27  \w     67.00 176.00   1.00   16.00    --  100.00  77.00 150.00  109
 28  \w     71.00 172.00   1.00   16.00    --  100.00  61.00-120.00  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      0.0424891000
_diffrn_orient_matrix_UB_12      -0.1640763000
_diffrn_orient_matrix_UB_13      -0.0171093000
_diffrn_orient_matrix_UB_21      0.1648179000
_diffrn_orient_matrix_UB_22      -0.0198387000
_diffrn_orient_matrix_UB_23      -0.0127765000
_diffrn_orient_matrix_UB_31      0.0334378000
_diffrn_orient_matrix_UB_32      -0.0469369000
_diffrn_orient_matrix_UB_33      0.0717120000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32547
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.600
_diffrn_reflns_theta_min         4.295
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.128
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.428
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       prism
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.00051(12)
_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   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0479P)^2^+0.6919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0904
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6492
_reflns_number_total             6766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05320_si_002.cif
_cod_data_source_block           Complex3
_cod_original_cell_volume        1788.37(9)
_cod_database_code               4127417
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C29 H45 B Co N7 O3 C4 H6 N2'
_reflns_odcompleteness_completeness 99.97
_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), C33(H33A,H33B,H33C)
;
_olex2_date_sample_data_collection 2019-03-16
_olex2_date_sample_submission    2019-03-15
_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 2.632
_oxdiff_exptl_absorpt_empirical_full_min 0.748