Exploring Steric Effects in Diastereoselective Synthesis of Chiral Aminophenolate Zinc Complexes and Stereoselective Ring-Opening Polymerization of rac-Lactide.
Wang, Haobing; Yang, Yang; Ma, Haiyan; Inorganic chemistry 55 (2016) 7356–7372; doi:10.1021/acs.inorgchem.6b00378

data_4347599
_publ_section_title
;
 Exploring Steric Effects in Diastereoselective Synthesis of Chiral
 Aminophenolate Zinc Complexes and Stereoselective Ring-Opening
 Polymerization of rac-Lactide.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7356
_journal_page_last               7372
_journal_paper_doi               10.1021/acs.inorgchem.6b00378
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_sum            'C41 H59 Cl2 N3 O Si2 Zn'
_chemical_formula_weight         802.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5402(10)
_cell_length_b                   18.245(2)
_cell_length_c                   24.821(3)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      29.50
_cell_measurement_theta_min      2.29
_cell_volume                     4320.4(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            42689
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.460
_diffrn_reflns_theta_min         1.385
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
; 
 Flack x determined using 4662 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.003(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         13110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0282P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0684
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                11464
_reflns_number_total             13110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00378_si_001.cif
_cod_data_source_block           mo_dm13049_0m
_cod_database_code               4347599
_shelx_estimated_absorpt_t_min   0.799
_shelx_estimated_absorpt_t_max   0.933
_shelxl_version_number           2013-4
_shelx_res_checksum              51442
_shelx_hkl_checksum              34306