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_4344765
_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_formula_moiety         'C38 H49 Na O6'
_chemical_formula_sum            'C38 H49 Na O6'
_chemical_formula_weight         624.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2015-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                108.317(9)
_cell_angle_beta                 96.963(7)
_cell_angle_gamma                101.806(8)
_cell_formula_units_Z            2
_cell_length_a                   11.0496(10)
_cell_length_b                   12.0612(12)
_cell_length_c                   14.4233(13)
_cell_measurement_reflns_used    3951
_cell_measurement_temperature    290.92(10)
_cell_measurement_theta_max      69.6210
_cell_measurement_theta_min      6.1750
_cell_volume                     1750.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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_temperature      290.92(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
  1 omega  -12.00   24.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000    0.0000 24

  2 omega   32.00   68.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000    0.0000 24

  3 omega  -68.00    8.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000 -120.0000 51

  4 omega   32.00  122.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -30.0000 60

  5 omega   26.00   77.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000 -180.0000 34

  6 omega   14.00   47.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   30.0000 22

  7 omega    7.00  122.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   19.0000  120.0000 77

  8 omega   38.00   63.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -180.0000 17

  9 omega   30.00  106.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000   30.0000 51

 10 omega  -15.00   75.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000 -180.0000 60

 11 omega   68.00  173.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000  -30.0000 70

 12 omega   56.00   89.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -90.0000 22

 13 omega   64.00   91.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000 -180.0000 18

 14 omega   41.00   78.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   60.0000 25

 15 omega   40.00  128.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -91.0000  120.0000 59

 16 omega   42.00  108.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   90.0000 44

 17 omega   64.00   91.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -60.0000 18

 18 omega   36.00   72.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000    0.0000 24

 19 omega   85.00  112.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 18

 20 omega   45.00   97.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -90.0000 35

 21 omega  100.00  124.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -63.0000  -30.0000 16

 22 omega   36.00   75.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -91.0000  -90.0000 26

 23 omega  106.00  134.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -91.0000  -90.0000 19

 24 omega   48.00   87.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  150.0000 26

 25 omega  105.00  174.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000 -180.0000 46

 26 omega   36.00  108.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -30.0000 48

 27 omega   37.00   89.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  120.0000 35

 28 omega  100.00  178.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000 -120.0000 52
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0494683000
_diffrn_orient_matrix_UB_12      0.1363871000
_diffrn_orient_matrix_UB_13      0.0596334000
_diffrn_orient_matrix_UB_21      0.1047951000
_diffrn_orient_matrix_UB_22      -0.0251135000
_diffrn_orient_matrix_UB_23      0.0651167000
_diffrn_orient_matrix_UB_31      0.0877566000
_diffrn_orient_matrix_UB_32      0.0125123000
_diffrn_orient_matrix_UB_33      -0.0734022000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11457
_diffrn_reflns_theta_full        69.66
_diffrn_reflns_theta_max         69.66
_diffrn_reflns_theta_min         4.00
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6439
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0668
_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^)+(0.1012P)^2^+1.4443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1831
_refine_ls_wR_factor_ref         0.1977
_reflns_number_gt                5232
_reflns_number_total             6439
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02709_si_004.cif
_cod_data_source_block           sunyy1224_red
_cod_database_code               4344765
_reflns_odcompleteness_completeness 99.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.023) H5(0.024) H22A(0.05) H22B(0.05) H22C(0.05) H23A(0.046)
 H23B(0.046) H23C(0.046) H24A(0.046) H24B(0.046) H24C(0.046) H28A(0.114)
 H28B(0.114) H28C(0.114) H27A(0.093) H27B(0.093) H27C(0.093) H26A(0.144)
 H26B(0.144) H26C(0.144) H9(0.029) H10(0.035) H11(0.036) H12(0.033) H14(0.027)
 H16(0.03) H17(0.035) H18(0.035) H19(0.029) H29A(0.074) H29B(0.074) H30A(0.072)
 H30B(0.072) H31A(0.078) H31B(0.078) H32A(0.084) H32B(0.084) H33A(0.092)
 H33B(0.092) H34A(0.102) H34B(0.102) H35A(0.092) H35B(0.092) H36A(0.091)
 H36B(0.091) H37A(0.09) H37B(0.09) H38A(0.09) H38B(0.09)
 Fixed X: H3(-0.0074) H5(-0.1831) H22A(0.1715) H22B(0.2787) H22C(0.1401)
 H23A(0.3474) H23B(0.4023) H23C(0.2937) H24A(0.2225) H24B(0.3588) H24C(0.3035)
 H28A(-0.3504) H28B(-0.2069) H28C(-0.2868) H27A(-0.197) H27B(-0.161) H27C(-
 0.3023) H26A(-0.3649) H26B(-0.3277) H26C(-0.423) H9(0.0603) H10(0.079)
 H11(0.0449) H12(-0.0099) H14(-0.0578) H16(-0.0953) H17(-0.1032) H18(-0.0655)
 H19(-0.0245) H29A(0.3648) H29B(0.4463) H30A(0.6272) H30B(0.5736) H31A(0.6856)
 H31B(0.6993) H32A(0.6817) H32B(0.56) H33A(0.6351) H33B(0.6685) H34A(0.5537)
 H34B(0.4385) H35A(0.3114) H35B(0.4219) H36A(0.4371) H36B(0.2978) H37A(0.2268)
 H37B(0.3744) H38A(0.2973) H38B(0.2368)
 Fixed Y: H3(0.1613) H5(0.4241) H22A(0.1112) H22B(0.1205) H22C(0.1112)
 H23A(0.4139) H23B(0.3018) H23C(0.2949) H24A(0.2955) H24B(0.3013) H24C(0.414)
 H28A(0.0326) H28B(0.0557) H28C(0.1371) H27A(0.1599) H27B(0.0637) H27C(0.0498)
 H26A(0.2785) H26B(0.2896) H26C(0.1722) H9(0.5518) H10(0.6559) H11(0.8496)
 H12(0.9353) H14(0.9249) H16(0.9216) H17(0.8266) H18(0.6347) H19(0.5391)
 H29A(0.6182) H29B(0.709) H30A(0.7256) H30B(0.5916) H31A(0.5593) H31B(0.689)
 H32A(0.5566) H32B(0.4706) H33A(0.6688) H33B(0.7588) H34A(0.8312) H34B(0.7192)
 H35A(0.8455) H35B(0.9598) H36A(1.0174) H36B(1.0039) H37A(0.937) H37B(0.9831)
 H38A(0.8437) H38B(0.7451)
 Fixed Z: H3(0.1661) H5(0.2417) H22A(0.1894) H22B(0.1281) H22C(0.0804)
 H23A(0.3057) H23B(0.2658) H23C(0.326) H24A(0.0421) H24B(0.0923) H24C(0.1272)
 H28A(0.0694) H28B(0.0643) H28C(0.0345) H27A(0.3211) H27B(0.2347) H27C(0.2454)
 H26A(0.1661) H26B(0.2776) H26C(0.2011) H9(0.0994) H10(-0.0077) H11(0.0348)
 H12(0.1825) H14(0.3426) H16(0.5071) H17(0.6212) H18(0.5839) H19(0.4321)
 H29A(0.4625) H29B(0.566) H30A(0.4909) H30B(0.4851) H31A(0.3454) H31B(0.3391)
 H32A(0.1806) H32B(0.1896) H33A(0.0815) H33B(0.1926) H34A(0.0839) H34B(0.063)
 H35A(0.1431) H35B(0.1597) H36A(0.3321) H36B(0.282) H37A(0.4323) H37B(0.4657)
 H38A(0.5404) H38B(0.4344)
;
_olex2_submission_special_instructions 'No special instructions were received'