Stereoselective Alkali-Metal Catalysts for Highly Isotactic Poly(rac-lactide) Synthesis.
Sun, Yangyang; Xiong, Jiao; Dai, Zhongran; Pan, Xiaobo; Tang, Ning; Wu, Jincai; Inorganic chemistry 55 (2015) 136–; doi:10.1021/acs.inorgchem.5b02709

data_4344767
_publ_section_title
;
 Stereoselective Alkali-Metal Catalysts for Highly Isotactic
 Poly(rac-lactide) Synthesis.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              136
_journal_paper_doi               10.1021/acs.inorgchem.5b02709
_journal_volume                  55
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C33 H39 K O8'
_chemical_formula_sum            'C33 H39 K O8'
_chemical_formula_weight         602.74
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.300(2)
_cell_length_b                   10.7796(7)
_cell_length_c                   14.2425(8)
_cell_measurement_reflns_used    1551
_cell_measurement_temperature    173.73(10)
_cell_measurement_theta_max      20.2820
_cell_measurement_theta_min      3.5420
_cell_volume                     3116.6(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      173.73(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_details
;
  1 omega  -12.00   22.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000  120.0000 34

  2 omega    0.00   84.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   57.0000    0.0000 84

  3 omega   -1.00   88.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   38.0000  -90.0000 89

  4 omega   19.00   44.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -77.0000 -120.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0016407000
_diffrn_orient_matrix_UB_12      0.0656598000
_diffrn_orient_matrix_UB_13      -0.0022329000
_diffrn_orient_matrix_UB_21      0.0338600000
_diffrn_orient_matrix_UB_22      0.0023094000
_diffrn_orient_matrix_UB_23      -0.0119160000
_diffrn_orient_matrix_UB_31      -0.0082797000
_diffrn_orient_matrix_UB_32      -0.0036886000
_diffrn_orient_matrix_UB_33      -0.0483667000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_unetI/netI     0.1253
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13468
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.89
_diffrn_reflns_theta_min         3.49
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_preparation       'toluene solution'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.41(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6344
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1374
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                3541
_reflns_number_total             6344
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02709_si_003.cif
_cod_data_source_block           sunyy0331_2
_cod_database_code               4344767
_chemical_oxdiff_formula         'C44 H28 S8'
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C30(H30A,H30B), C29(H29A,H29B), C31(H31A,H31B), C32(H32A,
 H32B), C23(H23A,H23B), C27(H27A,H27B), C22(H22A,H22B), C28(H28A,H28B),
 C25(H25A,H25B), C26(H26A,H26B), C24(H24A,H24B)
2.b Me refined with riding coordinates:
 C21(H21A,H21B,H21C)
2.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C9(H9), C3(H3), C14(H14), C16(H16), C12(H12), C5(H5), C2(H2),
 C17(H17), C10(H10), C11(H11), C18(H18)
;
_olex2_date_sample_data_collection 2015-03-31
_olex2_submission_special_instructions 'No special instructions were received'