Copper(I)/S8 Reversible Reactions Leading to an End-On Bound Dicopper(II) Disulfide Complex: Nucleophilic Reactivity and Analogies to Copper-Dioxygen Chemistry
Debabrata Maiti; Julia S. Woertink; Michael A. Vance; Ashley E. Milligan; Amy A. Narducci Sarjeant; Edward I. Solomon; Kenneth D. Karlin; Journal of the American Chemical Society 129 (2007) 8882–8892; doi:10.1021/ja071968z

data_4109662
_publ_section_title
;
 Copper(I)/S8 Reversible Reactions Leading to an End-On Bound Dicopper(II)
 Disulfide Complex: Nucleophilic Reactivity and Analogies to
 Copper-Dioxygen Chemistry
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8882
_journal_page_last               8892
_journal_paper_doi               10.1021/ja071968z
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C20 H22 Cu N4 O, C24 B F20'
_chemical_formula_sum            'C44 H22 B Cu F20 N4 O'
_chemical_formula_weight         1077.01
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_primary     direct
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_audit_creation_date
;
'Thu Jan 04 11:18:40 2007'
;
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.420(6)
_cell_angle_beta                 76.793(9)
_cell_angle_gamma                81.588(12)
_cell_formula_units_Z            2
_cell_length_a                   11.180(2)
_cell_length_b                   12.7666(12)
_cell_length_c                   14.9496(8)
_cell_measurement_reflns_used    13038
_cell_measurement_theta_max      27.9990
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_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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      0.0133927071
_diffrn_orient_matrix_UB_12      0.0098494125
_diffrn_orient_matrix_UB_13      -0.0488400579
_diffrn_orient_matrix_UB_21      -0.0611099756
_diffrn_orient_matrix_UB_22      0.0254087059
_diffrn_orient_matrix_UB_23      0.0015821882
_diffrn_orient_matrix_UB_31      0.0198633000
_diffrn_orient_matrix_UB_32      0.0493734386
_diffrn_orient_matrix_UB_33      0.0031891978
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
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_diffrn_reflns_number            25168
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_diffrn_reflns_theta_full        27.88
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_diffrn_source_voltage           50
_diffrn_standards_interval_count 2
_diffrn_standards_interval_time  50
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.822
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;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
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            orange
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.5231
_exptl_crystal_size_mid          0.2272
_exptl_crystal_size_min          0.1016
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         9677
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+2.0068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1352
_reflns_number_gt                7248
_reflns_number_total             9677
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja071968zsi20070320_115933.cif
_cod_data_source_block           x0326
_cod_original_cell_volume        2044.2(5)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4109662
_audit_creation_method_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection_reference
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_cell_refinment_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_cell_measurement_resolution_max 0.76
_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          x0326
_jhu_xray_labbook                II-47
_jhu_crystalization_labbook
;
;
_jhu_crystalization_solvent      'Ether, Pentane'
_jhu_crystalization_method
;
;
_jhu_diffraction_detector_distance 50
_jhu_quality_factor              2