Reactivity Study of a Hydroperoxodicopper(II) Complex: Hydroxylation, Dehydrogenation, and Ligand Cross-Link Reactions
Li, Lei; Sarjeant, Amy A. Narducci; Karlin, Kenneth D.; Inorganic Chemistry 45 (2006) 7160–7172; doi:10.1021/ic060598x

data_4332636
_publ_section_title
;
 Reactivity Study of a Hydroperoxodicopper(II) Complex:&#x00A0;
 Hydroxylation, Dehydrogenation, and Ligand Cross-Link Reactions
;
_journal_issue                   18
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7160
_journal_page_last               7172
_journal_paper_doi               10.1021/ic060598x
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C68 H72 Cu4 N12 O4, 6(C2 H3 N), 4(Cl O4)'
_chemical_formula_sum            'C80 H90 Cl4 Cu4 N18 O20'
_chemical_formula_weight         2019.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Wed Mar 22 17:37:08 2006'
;
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.197(8)
_cell_angle_beta                 109.379(9)
_cell_angle_gamma                100.108(7)
_cell_formula_units_Z            1
_cell_length_a                   11.9993(10)
_cell_length_b                   13.4080(11)
_cell_length_c                   16.1375(17)
_cell_measurement_reflns_used    5981
_cell_measurement_temperature    110
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      3.71
_cell_volume                     2246.7(4)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      'see scan set'
_diffrn_measurement_device       Kappa
_diffrn_measurement_device_type  Xcalibur3
_diffrn_measurement_method       ' omega scans'
_diffrn_orient_matrix_UB_11      0.0274002664
_diffrn_orient_matrix_UB_12      0.0138970747
_diffrn_orient_matrix_UB_13      0.0496732571
_diffrn_orient_matrix_UB_21      0.0196521167
_diffrn_orient_matrix_UB_22      0.0557467175
_diffrn_orient_matrix_UB_23      0.0062139644
_diffrn_orient_matrix_UB_31      -0.0564523898
_diffrn_orient_matrix_UB_32      0.0061775923
_diffrn_orient_matrix_UB_33      0.0027518236
_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  0.0640
_diffrn_reflns_av_sigmaI/netI    0.1056
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21363
_diffrn_reflns_resolution_max    0.83
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.64
_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    1.13111
_exptl_absorpt_correction_T_max  0.92869
_exptl_absorpt_correction_T_min  0.82162
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET)
(compiled Jan 13 2006,17:25:00)
Analytical numeric absorption correction using a multifaceted crystal
        model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.13077
_exptl_crystal_size_mid          0.07446
_exptl_crystal_size_min          0.03234
_refine_diff_density_max         1.414
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         8173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1401
_reflns_number_gt                4756
_reflns_number_total             8173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060598xsup3.cif
_cod_data_source_block           x0108
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               4332636
_audit_creation_method_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET)
(compiled Jan 13 2006,17:25:00)
;
_computing_data_collection_reference
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET)
(compiled Jan 13 2006,17:25:00)
;
_computing_cell_refinment_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET)
(compiled Jan 13 2006,17:25:00)
;
_computing_data_reduction_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET)
(compiled Jan 13 2006,17:25:00)
;
_cell_measurement_resolution_max 0.76