Impact of Na- and K-C pi-interactions on the structure and binding of M3(sol)n(BINOLate)3Ln catalysts.
Wooten, Alfred J.; Carroll, Patrick J.; Walsh, Patrick J.; Organic letters 9 (2007) 3359–3362; doi:10.1021/ol0713234

data_1505481
_publ_section_title
;
 Impact of Na- and K-C pi-interactions on the structure and binding of
 M3(sol)n(BINOLate)3Ln catalysts.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              3359
_journal_page_last               3362
_journal_paper_doi               10.1021/ol0713234
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C538 H402 K18 N34 O38 Yb6'
_chemical_formula_weight         9693.31
_space_group_IT_number           145
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      145
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   26.793(3)
_cell_length_b                   26.793(3)
_cell_length_c                   55.967(5)
_cell_measurement_temperature    143(1)
_cell_volume                     34794(6)
_computing_data_collection       'CrystalClear (Rigaku, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       'phi and omega rotations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_sigmaI/netI    0.1039
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            67876
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    1.430
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4552
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             14802
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         2.684
_refine_diff_density_min         -1.310
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     5369
_refine_ls_number_reflns         46587
_refine_ls_number_restraints     7875
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          2.349
_refine_ls_shift/su_mean         0.121
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+12.6352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1861
_refine_ls_wR_factor_ref         0.2001
_reflns_number_gt                36646
_reflns_number_total             46587
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol0713234-file003.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        34795(6)
_cod_original_sg_symbol_H-M      'P32       '
_cod_database_code               1505481