Toward Stereoselective Lactide Polymerization Catalysts: Cationic Zinc Complexes Supported by a Chiral Phosphinimine Scaffold
Hongsui Sun; Jamie S. Ritch; Paul G. Hayes; Inorganic Chemistry 50 (2011) 8063–8072; doi:10.1021/ic201139b

data_4326145
_publ_section_title
;
 Toward Stereoselective Lactide Polymerization Catalysts: Cationic Zinc
 Complexes Supported by a Chiral Phosphinimine Scaffold
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8063
_journal_page_last               8072
_journal_paper_doi               10.1021/ic201139b
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C53 H49 B Cl2 N O P'
_chemical_formula_weight         828.61
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.683(2)
_cell_angle_beta                 88.606(2)
_cell_angle_gamma                83.530(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5058(16)
_cell_length_b                   11.3748(18)
_cell_length_c                   18.371(3)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.41
_cell_measurement_theta_min      2.26
_cell_volume                     2158.4(6)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_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  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31192
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.41
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.9557
_exptl_absorpt_correction_T_min  0.8998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, R. H. (1995) Acta Cryst. A51, 33-38'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
The unit cell of compound 12 contained a heavily disordered molecule of
CH2Cl2, for which no suitable model could be found. The electron density
associated with this fragment was removed using SQUEEZE (PLATON)
(Van Sluis and Spek, 1990), leaving voids of ca. 300 cubic angstroms.
;
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         9735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+0.8984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1387
_reflns_number_gt                8089
_reflns_number_total             9735
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201139b_si_002_6.cif
_cod_data_source_block           compound12
_cod_database_code               4326145