Localization and Delocalization in a Mixed-Valence Dicopper Helicate
John C. Jeffery; Thomas Riis-Johannessen; Callum J. Anderson; Christopher J. Adams; Adam Robinson; Stephen P. Argent; Michael D. Ward; Craig R. Rice; Inorganic Chemistry 46 (2007) 2417–2426; doi:10.1021/ic061504m

data_4307001
_publ_section_title
;
Localization and Delocalization in a Mixed-Valence Dicopper Helicate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2417
_journal_page_last               2426
_journal_paper_doi               10.1021/ic061504m
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C29 H21 Cl2 Cu N5 O10 S2'
_chemical_formula_weight         798.07
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.0750(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8162(2)
_cell_length_b                   12.9136(2)
_cell_length_c                   16.8236(2)
_cell_measurement_reflns_used    6498
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      140.022
_cell_measurement_theta_min      6.469
_cell_volume                     3137.22(8)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.865
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Frames, each covering 0.3 \% in \w'
_diffrn_radiation_monochromator  'Osmic ConFocal MaxFlux mirror optics'
_diffrn_radiation_source         '4.8 kW rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14802
_diffrn_reflns_theta_full        70.04
_diffrn_reflns_theta_max         70.04
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    4.388
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.541949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         5147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0525P)^2^+1.1691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0853
_reflns_number_gt                4577
_reflns_number_total             5147
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061504msi20060809_123651.cif
_cod_data_source_block           riis37m
_cod_original_cell_volume        3137.22(7)
_cod_database_code               4307001