The bridge towards a more stable and active side-on-peroxido (Cu<sub>2</sub><sup>II</sup>(µ-η<sup>2</sup>:η<sup>2</sup>-O<sub>2</sub>)) complex as a tyrosinase model system.
Dalhoff, Rosalie; Schmidt, Regina; Steeb, Lena; Rabatinova, Kristina; Witte, Matthias; Teeuwen, Simon; Benjamaâ, Salim; Hüppe, Henrika; Hoffmann, Alexander; Herres-Pawlis, Sonja; Faraday discussions 244 (2023) 134–153; doi:10.1039/d2fd00162d

data_1568167
_publ_section_title
;
 The bridge towards a more stable and active side-on-peroxido
 (Cu<sub>2</sub><sup>II</sup>(&#xb5;-&#x3b7;<sup>2</sup>:&#x3b7;<sup>2</sup>-O<sub>2</sub>))
 complex as a tyrosinase model system.
;
_journal_issue                   0
_journal_name_full               'Faraday discussions'
_journal_page_first              134
_journal_page_last               153
_journal_paper_doi               10.1039/d2fd00162d
_journal_volume                  244
_journal_year                    2023
_chemical_formula_moiety         'C42 H56 N10'
_chemical_formula_sum            'C42 H56 N10'
_chemical_formula_weight         700.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-11-16 deposited with the CCDC.	2022-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.68(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.621(4)
_cell_length_b                   16.428(3)
_cell_length_c                   11.715(2)
_cell_measurement_reflns_used    16601
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.38
_cell_measurement_theta_min      6.90
_cell_volume                     3960.4(13)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.144.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.0.0 (STOE, 2018)
X-Area LANA 1.72.3.0 (STOE, 2018)
;
_computing_molecular_graphics    SHELXTL
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.82, Darmstadt 2018
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
3756 frames, detector distance = 65 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10667
_diffrn_reflns_point_group_measured_fraction_full 0.667
_diffrn_reflns_point_group_measured_fraction_max 0.667
_diffrn_reflns_theta_full        65.073
_diffrn_reflns_theta_max         65.073
_diffrn_reflns_theta_min         5.218
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_T_max  0.9054
_exptl_absorpt_correction_T_min  0.0123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.2(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         4519
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0572P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.384
_reflns_Friedel_fraction_full    0.371
_reflns_Friedel_fraction_max     0.371
_reflns_number_gt                3703
_reflns_number_total             4519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2fd00162d2.cif
_cod_data_source_block           L1
_cod_depositor_comments
'Adding full bibliography for 1568167--1568173.cif.'
_cod_original_cell_volume        3960.6(14)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1568167
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.926
_shelx_estimated_absorpt_t_max   0.946
_shelx_res_checksum              88552