Synthesis and Catalytic Activity of Heterobimetallic Rare Earth‒Zinc Ethyl BINOLate Analogues of Shibasaki’s Catalysts
Nieto, Ismael; Wooten, Alfred J.; Robinson, Jerome R.; Carroll, Patrick J.; Schelter, Eric J.; Walsh, Patrick J.; Organometallics 32 (2013) 7431–; doi:10.1021/om4009444

data_4082153
_publ_section_title
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 Synthesis and Catalytic Activity of Heterobimetallic Rare Earth--Zinc
 Ethyl BINOLate Analogues of Shibasaki&#x2019;s Catalysts
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_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7431
_journal_paper_doi               10.1021/om4009444
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C78 H75 O9 Pr Zn3'
_chemical_formula_weight         1493.40
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.173(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.9416(9)
_cell_length_b                   22.9328(18)
_cell_length_c                   12.2427(10)
_cell_measurement_temperature    143(1)
_cell_volume                     3352.0(5)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            88665
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    1.833
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     842
_refine_ls_number_reflns         15279
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0174
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+0.9264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0428
_reflns_number_gt                14774
_reflns_number_total             15279
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4009444_si_002.cif
_cod_data_source_block           shelxl_S_1_Pr
_cod_depositor_comments
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The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
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_cod_original_sg_symbol_H-M      'P 21     '
_cod_database_code               4082153