Formally Copper(III)-Alkylperoxo Complexes as Models of Possible Intermediates in Monooxygenase Enzymes.
Neisen, Benjamin D.; Gagnon, Nicole L.; Dhar, Debanjan; Spaeth, Andrew D.; Tolman, William B.; Journal of the American Chemical Society 139 (2017) 10220–10223; doi:10.1021/jacs.7b05754

data_4131483
_publ_section_title
;
 Formally Copper(III)-Alkylperoxo Complexes as Models of Possible
 Intermediates in Monooxygenase Enzymes.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10220
_journal_page_last               10223
_journal_paper_doi               10.1021/jacs.7b05754
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         0.5(C35H46CuN3O4,0.5(O1),0.5(C8H20N)
_chemical_formula_sum            'C21.5 H33 Cu0.5 N2 O2.5'
_chemical_formula_weight         391.27
_chemical_name_common            '[LCu(OOtBu)][NEt4]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.8830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9539(2)
_cell_length_b                   13.0791(2)
_cell_length_c                   15.0451(3)
_cell_measurement_reflns_used    9873
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      148.823
_cell_measurement_theta_min      6.759
_cell_volume                     2152.74(7)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX III Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    Shelxt
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Photon 100 CMOS'
_diffrn_measurement_method       '\ f and \ w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            47274
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.621
_diffrn_reflns_theta_min         3.379
_diffrn_source                   micro
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       block
_exptl_crystal_F_000             842
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.7538
_exptl_transmission_factor_min   0.6421
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1004P)^2^+0.9947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3814
_reflns_number_total             4409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b05754_si_003.cif
_cod_data_source_block           16213final_a
_cod_depositor_comments
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The following automatic conversions were performed:

data name '__diffrn_source' was replaced with '_diffrn_source'.

Automatic conversion script
Id: cif_correct_tags 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_original_formula_sum        'C21.50 H33 Cu0.50 N2 O2.50'
_cod_database_code               4131483
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              72018
_shelx_hkl_checksum              16625
_vrf_plat430_alert_2_a
; 
PROBLEM: Short Inter D...A Contact O4 .. O4 .. 1.97 Ang.
RESPONSE: O4 is a ha  
PROBLEM: Atom C13 has ADP max/min Ratio ..... 3.3 prolat
RESPONSE: C13 is a methyl carbon off of an isopropyl group with long ellipsoid most likely due to a wagging motion of methyl group.
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