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_1505480
_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            'C97.5 H73.5 Li3 N7.5 O6 Yb'
_chemical_formula_weight         1640.00
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      18
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9880(6)
_cell_length_b                   31.6872(10)
_cell_length_c                   14.5672(5)
_cell_measurement_temperature    143(1)
_cell_volume                     8303.1(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0885
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            44360
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    1.186
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5724
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3352
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.851
_refine_diff_density_min         -1.726
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.023(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1040
_refine_ls_number_reflns         18914
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1524
_reflns_number_gt                15847
_reflns_number_total             18914
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol0713234-file002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;

2019-04-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C195 H147 Li6 N15 O12 Yb2'
_cod_original_formula_weight         3280.00
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 21 21 2 '
_cod_database_code               1505480