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_4127414
_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
'C59 H56 B Co N7 O, 0.77(Cl), 0.18(C1 H2 Cl2), 0.82(C2 H3 N)'
_chemical_formula_sum            'C60.82 H58.82 B Cl1.13 Co N7.82 O'
_chemical_formula_weight         1025.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.8434(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.04169(13)
_cell_length_b                   31.9979(3)
_cell_length_c                   17.15695(14)
_cell_measurement_reflns_used    19799
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.3320
_cell_measurement_theta_min      4.6400
_cell_volume                     5447.22(10)
_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  'XL (Sheldrick, 2008)'
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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   -114.00 -14.00   1.00   11.00    --  -42.33 -57.00-120.00  100
  2  \w    -75.00  34.00   1.00   11.00    --  -42.33  77.00   0.00  109
  3  \w     23.00  98.00   1.00   11.00    --   42.33-125.00-180.00   75
  4  \w     74.00 173.00   1.00   45.00    --  100.00  45.00 120.00   99
  5  \w     74.00 173.00   1.00   45.00    --  100.00  45.00-180.00   99
  6  \w     27.00 126.00   1.00   45.00    --  100.00 -45.00 -30.00   99
  7  \w     94.00 173.00   1.00   45.00    --  100.00 125.00   0.00   79
  8  \w     28.00 129.00   1.00   45.00    --  100.00 -61.00  30.00  101
  9  \w     94.00 173.00   1.00   45.00    --  100.00 125.00 -30.00   79
 10  \w     28.00 129.00   1.00   45.00    --  100.00 -61.00 -30.00  101
 11  \w     17.00 109.00   1.00   45.00    --  100.00 -94.00 -90.00   92
 12  \w   -114.00 -14.00   1.00   11.00    --  -42.33 -57.00  30.00  100
 13  \w   -118.00 -10.00   1.00   11.00    --  -42.33 -77.00 150.00  108
 14  \w   -117.00 -18.00   1.00   11.00    --  -42.33 -37.00 -60.00   99
 15  \w     47.00 178.00   1.00   45.00    --  100.00  15.00 -30.00  131
;
_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      0.0822142000
_diffrn_orient_matrix_UB_12      -0.0155319000
_diffrn_orient_matrix_UB_13      -0.0630364000
_diffrn_orient_matrix_UB_21      -0.1316941000
_diffrn_orient_matrix_UB_22      -0.0082697000
_diffrn_orient_matrix_UB_23      -0.0568754000
_diffrn_orient_matrix_UB_31      0.0042720000
_diffrn_orient_matrix_UB_32      0.0448118000
_diffrn_orient_matrix_UB_33      -0.0323353000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            49988
_diffrn_reflns_theta_full        70.59
_diffrn_reflns_theta_max         70.59
_diffrn_reflns_theta_min         3.80
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.353
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.405
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2151
_exptl_crystal_size_max          0.387
_exptl_crystal_size_mid          0.278
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         10306
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+7.5357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1324
_reflns_number_gt                9555
_reflns_number_total             10306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9b05320_si_002.cif
_cod_data_source_block           Complex1
_cod_database_code               4127414
_chemical_oxdiff_formula         'Co C53 H44 N7 O B C2 H3 N C H2 Cl2'
_reflns_odcompleteness_completeness 99.91
_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, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 N8, C60, C61
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Sof(Cl2)=Sof(Cl1)=0.5*FVAR(2)
 Sof(N8)=Sof(C60)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=1-FVAR(2)
 Sof(Cl3)=Sof(Cl4)=Sof(C62)=Sof(H62A)=Sof(H62B)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 B1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C62(H62A,H62B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C8(H8), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25),
  C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43),
  C44(H44), C45(H45), C48(H48), C50(H50)
4.d Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C61(H61A,H61B,H61C)
;
_olex2_date_sample_data_collection 2017-07-21
_olex2_date_sample_submission    2017-07-20
_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 3.153
_oxdiff_exptl_absorpt_empirical_full_min 0.681