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_4127416
_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 H44 B Co N7 O, 3(C2 H3 N)'
_chemical_formula_sum            'C35 H53 B Co N10 O'
_chemical_formula_weight         699.61
_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             2017-07-14
_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                 96.6314(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.63615(4)
_cell_length_b                   18.95826(9)
_cell_length_c                   26.67111(12)
_cell_measurement_reflns_used    19060
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.7880
_cell_measurement_theta_min      4.0560
_cell_volume                     3835.29(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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   -130.00 -79.00   0.50    4.00    --  -34.31 -99.00  60.00  102
  2  \w   -130.00 -79.00   0.50    4.00    --  -34.31 -99.00-150.00  102
  3  \w   -130.00 -79.00   0.50    4.00    --  -34.31 -99.00-180.00  102
  4  \w   -130.00 -79.00   0.50    4.00    --  -34.31 -99.00 -30.00  102
  5  \w   -127.00 -73.00   0.50    4.00    --  -34.31-125.00   0.00  108
  6  \w    -81.00  33.00   0.50    4.00    --  -34.31  88.00-119.00  228
  7  \w   -130.00 -79.00   0.50    4.00    --  -34.31 -99.00   0.00  102
  8  \w   -127.00 -73.00   0.50    4.00    --  -34.31-125.00 120.00  108
  9  \w     23.00 101.00   0.50    4.00    --   34.31-125.00  90.00  156
 10  \w    100.00 178.00   0.50    8.00    --  100.00 111.00 -90.00  156
 11  \w    100.00 178.00   0.50    8.00    --  100.00 111.00   0.00  156
 12  \w     12.00 115.00   0.50    8.00    --  100.00-111.00-150.00  206
 13  \w     14.00 178.00   0.50    8.00    --  100.00  25.00 -90.00  328
 14  \w     57.00 178.00   0.50    8.00    --  100.00  66.00  43.05  242
 15  \w     12.00 115.00   0.50    8.00    --  100.00-111.00  30.00  206
 16  \w     57.00 150.00   0.50    8.00    --  100.00 178.00 120.00  186
 17  \w     57.00 150.00   0.50    8.00    --  100.00 178.00-120.00  186
 18  \w    100.00 178.00   0.50    8.00    --  100.00 111.00 -30.00  156
 19  \w     69.00 168.00   0.50    8.00    --  100.00  50.00 -60.00  198
 20  \w     99.00 178.00   0.50    8.00    --  100.00  88.00-119.00  158
 21  \w    101.00 150.00   0.50    8.00    --  100.00 111.00  90.00   98
;
_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      0.0249016000
_diffrn_orient_matrix_UB_12      -0.0731396000
_diffrn_orient_matrix_UB_13      0.0249771000
_diffrn_orient_matrix_UB_21      -0.1979830000
_diffrn_orient_matrix_UB_22      -0.0023681000
_diffrn_orient_matrix_UB_23      0.0062701000
_diffrn_orient_matrix_UB_31      -0.0380017000
_diffrn_orient_matrix_UB_32      -0.0353371000
_diffrn_orient_matrix_UB_33      -0.0521261000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            26380
_diffrn_reflns_theta_full        65.86
_diffrn_reflns_theta_max         65.86
_diffrn_reflns_theta_min         3.34
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.823
_exptl_absorpt_correction_T_max  0.558
_exptl_absorpt_correction_T_min  0.271
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.459
_exptl_crystal_size_mid          0.388
_exptl_crystal_size_min          0.187
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         6623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+1.8405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0865
_reflns_number_gt                6563
_reflns_number_total             6623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9b05320_si_002.cif
_cod_data_source_block           Complex2
_cod_database_code               4127416
_chemical_oxdiff_formula         'Co C29 H44 N7 O B (C2 H3 N)3'
_reflns_odcompleteness_completeness 98.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.34
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All N(H,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 Secondary CH2 refined with riding coordinates:
 N7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C8(H8), C18(H18), C20(H20)
2.d 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), C35(H35A,H35B,H35C), C31(H31A,H31B,H31C), C33(H33A,H33B,
 H33C)
;
_olex2_date_sample_submission    2017-07-13
_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 1.393
_oxdiff_exptl_absorpt_empirical_full_min 0.569