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_7043545
_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_absolute_configuration ad
_chemical_formula_moiety         'C50 H44 B Co N7 O2 S'
_chemical_formula_sum            'C50 H44 B Co N7 O2 S'
_chemical_formula_weight         876.72
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_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                 91.5914(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.77282(13)
_cell_length_b                   16.76061(12)
_cell_length_c                   16.80269(14)
_cell_measurement_reflns_used    18759
_cell_measurement_temperature    99.95(10)
_cell_measurement_theta_max      74.0660
_cell_measurement_theta_min      3.6970
_cell_volume                     4440.28(6)
_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 0.9996
_diffrn_measured_fraction_theta_max 0.8944
_diffrn_measurement_details
;
  1 omega  -96.00   -2.00   1.0000    6.0450
omega____ theta____ kappa____ phi______ frames
    -      -41.6487  125.0000  -30.0000 94

  2 omega -120.00   -8.00   1.0000    6.0450
omega____ theta____ kappa____ phi______ frames
    -      -41.6487  -77.0000 -120.0000 112

  3 omega  -49.00   35.00   1.0000    6.0450
omega____ theta____ kappa____ phi______ frames
    -      -41.6487   37.0000  120.0000 84

  4 omega   94.00  178.00   1.0000   24.1800
omega____ theta____ kappa____ phi______ frames
    -      108.2878  125.0000    0.0000 84

  5 omega   30.00   90.00   1.0000   24.1800
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -30.0000  120.0000 60

  6 omega   24.00  109.00   1.0000   24.1800
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -94.0000  -90.0000 85

  7 omega   30.00   90.00   1.0000   24.1800
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -30.0000 -150.0000 60

  8 omega   81.00  178.00   1.0000   24.1800
omega____ theta____ kappa____ phi______ frames
    -      108.2878   45.0000 -150.0000 97

  9 omega   33.00  122.00   1.0000   24.1800
omega____ theta____ kappa____ phi______ frames
    -      108.2878 -125.0000   60.0000 89

 10 omega   94.00  178.00   1.0000   24.1800
omega____ theta____ kappa____ phi______ frames
    -      108.2878  125.0000 -120.0000 84

 11 omega   34.00   98.00   1.0000   24.1800
omega____ theta____ kappa____ phi______ frames
    -      108.2878  -45.0000  -30.0000 64

 12 omega -124.00  -79.00   1.0000    6.0450
omega____ theta____ kappa____ phi______ frames
    -      -41.6487  -99.0000    0.0000 45

 13 omega -118.00  -15.00   1.0000    6.0450
omega____ theta____ kappa____ phi______ frames
    -      -41.6487  -37.0000   90.0000 103

 14 omega -116.00  -12.00   1.0000    6.0450
omega____ theta____ kappa____ phi______ frames
    -      -41.6487  -57.0000    0.0000 104

 15 omega   78.00  178.00   1.0000   24.1800
omega____ theta____ kappa____ phi______ frames
    -      108.2878   30.0000   30.0000 100

 16 omega   78.00  178.00   1.0000   24.1800
omega____ theta____ kappa____ phi______ frames
    -      108.2878   30.0000  -60.0000 100

 17 omega   75.00  178.00   1.0000   24.1800
omega____ theta____ kappa____ phi______ frames
    -      108.2878   77.0000  150.0000 103

 18 omega   78.00  125.00   1.0000   24.1800
omega____ theta____ kappa____ phi______ frames
    -      108.2878   61.0000   60.0000 47

 19 omega   81.00  178.00   1.0000   24.1800
omega____ theta____ kappa____ phi______ frames
    -      108.2878   45.0000  120.0000 97
;
_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      -0.0026875000
_diffrn_orient_matrix_UB_12      0.0908732000
_diffrn_orient_matrix_UB_13      -0.0137009000
_diffrn_orient_matrix_UB_21      0.0495247000
_diffrn_orient_matrix_UB_22      0.0130629000
_diffrn_orient_matrix_UB_23      0.0792497000
_diffrn_orient_matrix_UB_31      0.0841795000
_diffrn_orient_matrix_UB_32      -0.0047563000
_diffrn_orient_matrix_UB_33      -0.0440777000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40090
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         76.61
_diffrn_reflns_theta_min         3.73
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.851
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.784
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1828
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.4288
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.0553
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.021(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1124
_refine_ls_number_reflns         16708
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0946P)^2^+1.4148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1566
_reflns_number_gt                14231
_reflns_number_total             16708
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01600j2.cif
_cod_data_source_block           complex3
_cod_database_code               7043545
_chemical_oxdiff_formula         'Co C48 H44 B N7 O2 S'
_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, All C(H,H) groups, All C(H,H,H,H) groups,
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C50B) = Uanis(C50)
3. Others
 Sof(H49C)=Sof(H49D)=Sof(C50B)=Sof(H50D)=Sof(H50E)=Sof(H50F)=1-FVAR(1)
 Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C47(H47), B1(H1), C47A(H47A), B1A(H1A)
4.b Secondary CH2 refined with riding coordinates:
 N7(H7A,H7B), C46(H46A,H46B), C49(H49A,H49B), C49(H49C,H49D), N7A(H7AA,H7AB),
 C46A(H46C,H46D), C49A(H49E,H49F)
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), C2A(H2A), C5A(H5A), C8A(H8A), C11A(H11A), C12A(H12A),
 C13A(H13A), C14A(H14A), C15A(H15A), C17A(H17A), C18A(H18A), C19A(H19A),
 C20A(H20A), C21A(H21A), C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A),
 C27A(H27A), C29A(H29A), C30A(H30A), C31A(H31A), C32A(H32A), C33A(H33A),
 C35A(H35A), C36A(H36A), C37A(H37A), C38A(H38A), C39A(H39A), C41A(H41A),
 C42A(H42A), C43A(H43A), C44A(H44A), C45A(H45A)
4.d Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C50B(H50D,H50E,H50F), C50A(H50H,H50G,H50I)
;
_olex2_date_sample_data_collection 2016-11-29
_olex2_date_sample_submission    2016-11-29
_olex2_submission_special_instructions 'No special instructions were received'