Aryl Hydroxylation from a Mononuclear Copper-Hydroperoxo Species
Debabrata Maiti; Heather R. Lucas; Amy A. Narducci Sarjeant; Kenneth D. Karlin; Journal of the American Chemical Society 129 (2007) 6998–6999; doi:10.1021/ja071704c

data_4109488
_publ_section_title
;
 Aryl Hydroxylation from a Mononuclear Copper-Hydroperoxo Species
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6998
_journal_page_last               6999
_journal_paper_doi               10.1021/ja071704c
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C31 H36 Cl Cu N4 O5, Cl O4'
_chemical_formula_sum            'C31 H36 Cl2 Cu N4 O9'
_chemical_formula_weight         743.08
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Fri Jan 06 11:46:30 2006'
;
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.733(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.498(2)
_cell_length_b                   11.7373(7)
_cell_length_c                   17.080(2)
_cell_measurement_reflns_used    20346
_cell_measurement_temperature    110
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      1.81
_cell_volume                     3303.6(6)
_computing_cell_refinement       'Oxford Diffraction CrysAlis RED'
_computing_data_collection       'Oxford Diffraction CrysAlis CCD'
_computing_data_reduction        'Oxford Diffraction CrysAlis RED'
_computing_molecular_graphics    'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_computing_publication_material  'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_computing_structure_refinement  'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_computing_structure_solution    'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_diffrn_ambient_temperature      110
_diffrn_detector_area_resol_mean 15.9890
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      'see scan set'
_diffrn_measurement_device       Kappa
_diffrn_measurement_device_type  Xcalibur3
_diffrn_measurement_method       ' omega phi scans'
_diffrn_orient_matrix_UB_11      0.0247731333
_diffrn_orient_matrix_UB_12      0.0184607484
_diffrn_orient_matrix_UB_13      -0.0304387969
_diffrn_orient_matrix_UB_21      -0.0350465079
_diffrn_orient_matrix_UB_22      0.0068813346
_diffrn_orient_matrix_UB_23      -0.0253838116
_diffrn_orient_matrix_UB_31      -0.0037857079
_diffrn_orient_matrix_UB_32      0.0572107535
_diffrn_orient_matrix_UB_33      0.0128326014
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            48617
_diffrn_reflns_resolution_max    0.75
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.78
_diffrn_source_current           40
_diffrn_source_power             2
_diffrn_source_voltage           50
_diffrn_standards_interval_count 1
_diffrn_standards_interval_time  50
_exptl_absorpt_coefficient_mu    0.88225
_exptl_absorpt_correction_T_max  0.93161
_exptl_absorpt_correction_T_min  0.75288
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle7 beta (release 01-12-2005 CrysAlis171 .NET)
(compiled Dec  1 2005,15:12:38)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       plate
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.21846
_exptl_crystal_size_mid          0.12428
_exptl_crystal_size_min          0.03994
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         8164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0464P)^2^+1.1035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0820
_reflns_number_gt                6505
_reflns_number_total             8164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja071704csi20070311_111220.cif
_cod_data_source_block           x0182_Cu(II)(6tBP)(acetone)(ClO4)2_(1)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4109488
_audit_creation_method_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle7 beta (release 01-12-2005 CrysAlis171 .NET)
(compiled Dec  1 2005,15:12:38)
;
_computing_data_collection_reference
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.28cycle7 beta (release 01-12-2005 CrysAlis171 .NET)
(compiled Dec  1 2005,15:12:38)
;
_computing_cell_refinment_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle7 beta (release 01-12-2005 CrysAlis171 .NET)
(compiled Dec  1 2005,15:12:38)
;
_computing_data_reduction_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle7 beta (release 01-12-2005 CrysAlis171 .NET)
(compiled Dec  1 2005,15:12:38)
;
_cell_measurement_resolution_max 0.72
_jhu_your_name_here              'Dr. Amy A Sarjeant'
_jhu_your_lab_here               'NCB 240'
_jhu_your_phone_number_here      x6-8569
_jhu_your_email_here             xray@jhu.edu
_jhu_institutional_source        'Karlin Lab'
_jhu_submitting_scientist        'Debabrata Maiti'
_jhu_scientist_phone             x6-6557
_jhu_scientist_email             dmaiti1@jhu.edu
_jhu_identifying_number          x0182
_jhu_xray_labbook                123
_jhu_crystalization_labbook
;
;
_jhu_crystalization_solvent      'Acetonitrile, Ether'
_jhu_crystalization_method       Evaporation
_jhu_diffraction_detector_distance 50
_jhu_quality_factor              1