NOE and PGSE NMR Spectroscopic Studies of Solution Structure and Aggregation in Metallocenium Ion-Pairs
Cristiano Zuccaccia; Nicholas G. Stahl; Alceo Macchioni; Ming-Chou Chen; John A. Roberts; Tobin J. Marks; Journal of the American Chemical Society 126 (2004) 1448–1464; doi:10.1021/ja0387296

data_4112156
_publ_section_title
;
 NOE and PGSE NMR Spectroscopic Studies of Solution Structure and
 Aggregation in Metallocenium Ion-Pairs
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1448
_journal_page_last               1464
_journal_paper_doi               10.1021/ja0387296
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C17 H25 O Si Zr, C24 B F20, C6 H6'
_chemical_formula_sum            'C47 H31 B F20 O Si Zr'
_chemical_formula_weight         1121.84
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.515(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.037(3)
_cell_length_b                   16.263(3)
_cell_length_c                   18.351(3)
_cell_measurement_temperature    153(2)
_cell_volume                     4633.4(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1042
_diffrn_reflns_av_sigmaI/netI    0.0869
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37809
_diffrn_reflns_theta_full        28.47
_diffrn_reflns_theta_max         28.47
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_T_max  0.96566
_exptl_absorpt_correction_T_min  0.87164
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            'flat needle'
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_meas      0
_exptl_crystal_description       colorless
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.540
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.488
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         10806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+11.9176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1584
_reflns_number_gt                6273
_reflns_number_total             10806
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0387296si20030925_065121.cif
_cod_data_source_block           cricroz1
_cod_original_cell_volume        4633.2(14)
_cod_database_code               4112156