Probing Flexibility in Porphyrin-Based Molecular Wires Using Double Electron Electron Resonance
Janet E. Lovett; Markus Hoffmann; Arjen Cnossen; Alexander T. J. Shutter; Hannah J. Hogben; Christopher W. M. Kay; Christiane R. Timmel; Harry L. Anderson; Journal of the American Chemical Society 131 (2009) 13852–13859; doi:10.1021/ja905796z

data_4105082
_publ_contact_author_address
;
   Department of Chemistry
   University of Bath
   Claverton Down
   Bath
   BA2 7AY
   UK
;
_publ_contact_author_email       s.pascu@bath.ac.uk
_publ_contact_author_fax         '(01225) 386231'
_publ_contact_author_name        'Sofia I. Pascu'
_publ_contact_author_phone       '(01225) 386627'
_publ_section_title
;
 Probing Flexibility in Porphyrin-Based Molecular Wires Using Double
 Electron Electron Resonance
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13852
_journal_page_last               13859
_journal_paper_doi               10.1021/ja905796z
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C92 H108 N6 O10 Zn, 2(C4 H8 O2)'
_chemical_formula_sum            'C100 H124 N6 O14 Zn'
_chemical_formula_weight         1699.45
_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
_audit_creation_date             31-03-09
_audit_creation_method           CRYSTALS_ver_12.80
_cell_angle_alpha                68.881(5)
_cell_angle_beta                 89.920(5)
_cell_angle_gamma                89.596(5)
_cell_formula_units_Z            2
_cell_length_a                   12.691(5)
_cell_length_b                   19.134(7)
_cell_length_c                   20.044(7)
_cell_measurement_reflns_used    12203
_cell_measurement_temperature    120
_cell_measurement_theta_max      25
_cell_measurement_theta_min      0
_cell_volume                     4540(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD'
_diffrn_measurement_method       'fine-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6939
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19667
_diffrn_reflns_theta_full        22.155
_diffrn_reflns_theta_max         22.155
_diffrn_reflns_theta_min         1.232
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       needle
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.70
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.3046
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     850
_refine_ls_number_reflns         6880
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0730
_refine_ls_shift/su_max          0.006154
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.965 0.559 0.666 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1061
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0868
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              20
_reflns_limit_k_min              -19
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                6880
_reflns_number_total             12057
_reflns_threshold_expression     I>2.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.2012(6)
_cod_data_source_file            ja905796z_si_001.cif
_cod_data_source_block           bath721
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4105082