Direct Evidence for a Geometrically Constrained "Entatic State" Effect on Copper(II/I) Electron-Transfer Kinetics As Manifested in Metastable Intermediates
Qiuyue Yu; Cynthia A. Salhi; Edna A. Ambundo; Mary Jane Heeg; L. A. Ochrymowycz; D. B. Rorabacher; Journal of the American Chemical Society 123 (2001) 5720–5729; doi:10.1021/ja002995r

data_4115574
_publ_section_title
;
 Direct Evidence for a Geometrically Constrained "Entatic State" Effect on
 Copper(II/I) Electron-Transfer Kinetics As Manifested in Metastable
 Intermediates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5720
_journal_page_last               5729
_journal_paper_doi               10.1021/ja002995r
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C18 H34 Cl2 Cu O9 S4'
_chemical_formula_weight         657.13
_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_method           SHELXL
_cell_angle_alpha                96.0250(10)
_cell_angle_beta                 99.5220(10)
_cell_angle_gamma                117.543(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2133(8)
_cell_length_b                   10.3016(8)
_cell_length_c                   14.8454(12)
_cell_measurement_reflns_used    3180
_cell_measurement_temperature    295(2)
_cell_volume                     1336.10(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Bruker P4/CCD'
_diffrn_measurement_method       'SMART CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_av_sigmaI/netI    0.0673
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9259
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    1.375
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark_blue
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       plate
_exptl_crystal_F_000             682
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.0000(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.951
_refine_ls_goodness_of_fit_obs   1.076
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         5867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_restrained_S_obs      1.076
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_obs          0.0479
_refine_ls_shift/esd_max         -3.476
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1254
_refine_ls_wR_factor_obs         0.1052
_reflns_number_observed          3508
_reflns_number_total             5868
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja002995r_1.cif
_cod_data_source_block           Cu(II)L7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1336.1(2)
_cod_database_code               4115574