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_4115578
_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           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.7850(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5370(6)
_cell_length_b                   13.7475(7)
_cell_length_c                   17.7187(9)
_cell_measurement_reflns_used    7678
_cell_measurement_temperature    295(2)
_cell_volume                     2751.0(2)
_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  0.029
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19056
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    1.335
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.0000(4)
_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   1.034
_refine_ls_goodness_of_fit_obs   1.125
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         6420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_restrained_S_obs      1.125
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_obs          0.0529
_refine_ls_shift/esd_max         -2.557
_refine_ls_shift/esd_mean        0.027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+0.8123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1646
_refine_ls_wR_factor_obs         0.1471
_reflns_number_observed          4505
_reflns_number_total             6422
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja002995r_5.cif
_cod_data_source_block           Cu(II)L11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+0.8123P] 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^)+(0.0972P)^2^+0.8123P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4115578