Spectroscopic and computational studies of reversible O2 binding by a cobalt complex of relevance to cysteine dioxygenase.
Fischer, Anne A.; Lindeman, Sergey V.; Fiedler, Adam T.; Dalton transactions (Cambridge, England : 2003)  (2017) –; doi:10.1039/c7dt01600j

data_7043546
_publ_section_title
;
 Spectroscopic and computational studies of reversible O2 binding by a
 cobalt complex of relevance to cysteine dioxygenase.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/c7dt01600j
_journal_year                    2017
_chemical_formula_moiety         'C17 H25 B Co N6 O2'
_chemical_formula_sum            'C17 H25 B Co N6 O2'
_chemical_formula_weight         415.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-04-20 deposited with the CCDC.
2017-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.778(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7807(3)
_cell_length_b                   7.71018(14)
_cell_length_c                   18.8008(3)
_cell_measurement_reflns_used    10317
_cell_measurement_temperature    99.95(10)
_cell_measurement_theta_max      28.9660
_cell_measurement_theta_min      3.4390
_cell_volume                     1940.14(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      99.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_details
;
  1 omega -100.00  -55.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      -11.5916  178.0000  -60.0000 45

  2 omega  -20.00   30.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      -11.5916  -99.0000  150.0000 50

  3 omega  -62.00   41.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -       11.6697  -57.0000  120.0000 103

  4 omega  -62.00   41.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -       11.6697  -57.0000 -120.0000 103

  5 omega  -22.00   90.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -       11.6697   77.0000 -150.0000 112

  6 omega   34.00   71.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -       11.6697 -178.0000   90.0000 37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0092856000
_diffrn_orient_matrix_UB_12      0.0901469000
_diffrn_orient_matrix_UB_13      -0.0020004000
_diffrn_orient_matrix_UB_21      -0.0515844000
_diffrn_orient_matrix_UB_22      0.0172642000
_diffrn_orient_matrix_UB_23      -0.0039402000
_diffrn_orient_matrix_UB_31      0.0079202000
_diffrn_orient_matrix_UB_32      0.0064313000
_diffrn_orient_matrix_UB_33      0.0385767000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22252
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.54
_diffrn_reflns_theta_min         3.46
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.909
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.2565
_exptl_crystal_size_mid          0.2016
_exptl_crystal_size_min          0.1096
_refine_diff_density_max         1.041
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0715P)^2^+1.0520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1274
_reflns_number_gt                4160
_reflns_number_total             4939
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01600j2.cif
_cod_data_source_block           complex5
_cod_original_cell_volume        1940.14(6)
_cod_database_code               7043546
_chemical_oxdiff_formula         'Co C17 H24 B N6 O2'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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)
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), C17(H17A,H17B,H17C)
;
_olex2_date_sample_data_collection 2016-11-14
_olex2_date_sample_submission    2016-11-11
_olex2_submission_special_instructions 'No special instructions were received'