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_4109664
_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 Cl Cu N4 O, C24 B F20'
_chemical_formula_sum            'C44 H22 B Cl Cu F20 N4 O'
_chemical_formula_weight         1112.46
_chemical_name_systematic
; 
 ? 
;
_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
;
'Wed Mar 02 09:25:41 2005'
;
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.343(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4310(15)
_cell_length_b                   18.200(2)
_cell_length_c                   20.593(3)
_cell_measurement_reflns_used    5922
_cell_measurement_temperature    110
_cell_measurement_theta_max      23.30
_cell_measurement_theta_min      1.93
_cell_volume                     4227.4(10)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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      -0.0037663134
_diffrn_orient_matrix_UB_12      0.0260809406
_diffrn_orient_matrix_UB_13      -0.0257541824
_diffrn_orient_matrix_UB_21      -0.0468008961
_diffrn_orient_matrix_UB_22      -0.0202817880
_diffrn_orient_matrix_UB_23      -0.0183903480
_diffrn_orient_matrix_UB_31      -0.0416386527
_diffrn_orient_matrix_UB_32      0.0206144002
_diffrn_orient_matrix_UB_33      0.0144369552
_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  0.0556
_diffrn_reflns_av_sigmaI/netI    0.1004
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31190
_diffrn_reflns_resolution_max    0.75
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.81
_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    0.70748
_exptl_absorpt_correction_T_max  0.93765
_exptl_absorpt_correction_T_min  0.90644
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.26pre9 beta (release 04-02-2005 CrysAlis171 .NET)
(compiled Feb  4 2005,10:44:33)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       prism
_exptl_crystal_F_000             2212
_exptl_crystal_size_max          0.11407
_exptl_crystal_size_mid          0.07002
_exptl_crystal_size_min          0.03846
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         10463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0408P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                5854
_reflns_number_total             10463
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja071968zsi20070320_120010.cif
_cod_data_source_block           x0105
_cod_original_cell_volume        4227.5(10)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4109664
_audit_creation_method_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.26pre9 beta (release 04-02-2005 CrysAlis171 .NET)
(compiled Feb  4 2005,10:44:33)
;
_computing_data_collection_reference
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.26pre9 beta (release 04-02-2005 CrysAlis171 .NET)
(compiled Feb  4 2005,10:44:33)
;
_computing_cell_refinment_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.26pre9 beta (release 04-02-2005 CrysAlis171 .NET)
(compiled Feb  4 2005,10:44:33)
;
_computing_data_reduction_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.26pre9 beta (release 04-02-2005 CrysAlis171 .NET)
(compiled Feb  4 2005,10:44:33)
;
_cell_measurement_resolution_max 0.90
_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          x0105
_jhu_xray_labbook                77
_jhu_crystalization_labbook      6MeO-Cl
_jhu_crystalization_solvent
'Heptane, Tetrahydrofuran, Deuterated Chloroform, Pentane'
_jhu_crystalization_method       Evaporation
_jhu_diffraction_detector_distance 50
_jhu_quality_factor              2