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_4332634
_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         ' C70 H64 Cu2 N6 O P2, C4 H10 O, 2(Cl O4)'
_chemical_formula_sum            'C74 H74 Cl2 Cu2 N6 O10 P2'
_chemical_formula_weight         1467.31
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Fri Feb 11 09:27:39 2005'
;
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.608(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1565(8)
_cell_length_b                   14.3470(6)
_cell_length_c                   28.0808(12)
_cell_measurement_reflns_used    15744
_cell_measurement_temperature    110
_cell_measurement_theta_max      29.20
_cell_measurement_theta_min      1.78
_cell_volume                     7045.1(5)
_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       ' phi omega scans'
_diffrn_orient_matrix_UB_11      0.0009967974
_diffrn_orient_matrix_UB_12      -0.0082996300
_diffrn_orient_matrix_UB_13      0.0250598312
_diffrn_orient_matrix_UB_21      -0.0292386947
_diffrn_orient_matrix_UB_22      -0.0338823009
_diffrn_orient_matrix_UB_23      -0.0076112577
_diffrn_orient_matrix_UB_31      0.0280953826
_diffrn_orient_matrix_UB_32      -0.0350330453
_diffrn_orient_matrix_UB_33      0.0013774243
_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  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            85970
_diffrn_reflns_resolution_max    0.77
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.90
_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    0.78802
_exptl_absorpt_correction_T_max  0.92000
_exptl_absorpt_correction_T_min  0.77083
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.24 beta (release 23.09.2004 CrysAlis171 .NET)
(compiled Oct 19 2004,12:04:41)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.19658
_exptl_crystal_size_mid          0.12983
_exptl_crystal_size_min          0.04786
_refine_diff_density_max         1.210
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     936
_refine_ls_number_reflns         16106
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0816P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1430
_reflns_number_gt                11627
_reflns_number_total             16106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060598xsup1.cif
_cod_data_source_block           x0100
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'Analytical'
changed to 'analytical' 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      'P2(1)/c  '
_cod_database_code               4332634
_audit_creation_method_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.24 beta (release 23.09.2004 CrysAlis171 .NET)
(compiled Oct 19 2004,12:04:41)
;
_computing_data_collection_reference
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.24 beta (release 23.09.2004 CrysAlis171 .NET)
(compiled Oct 19 2004,12:04:41)
;
_computing_cell_refinment_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.24 beta (release 23.09.2004 CrysAlis171 .NET)
(compiled Oct 19 2004,12:04:41)
;
_computing_data_reduction_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.24 beta (release 23.09.2004 CrysAlis171 .NET)
(compiled Oct 19 2004,12:04:41)
;
_cell_measurement_resolution_max 0.73