Iso-Selective Ring-Opening Polymerization of rac-Lactide Catalyzed by Crown Ether Complexes of Sodium and Potassium Naphthalenolates.
Xiong, Jiao; Zhang, Jinjin; Sun, Yangyang; Dai, Zhongran; Pan, Xiaobo; Wu, Jincai; Inorganic chemistry 54 (2015) 1737–1743; doi:10.1021/ic502685f

data_4342283
_publ_section_title
;
 Iso-Selective Ring-Opening Polymerization of rac-Lactide Catalyzed by
 Crown Ether Complexes of Sodium and Potassium Naphthalenolates.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1737
_journal_page_last               1743
_journal_paper_doi               10.1021/ic502685f
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C39 H41 K O8'
_chemical_formula_sum            'C39 H41 K O8'
_chemical_formula_weight         676.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-05
_audit_creation_method
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Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
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_cell_length_a                   17.2945(3)
_cell_length_b                   14.4199(2)
_cell_length_c                   27.1372(4)
_cell_measurement_reflns_used    8852
_cell_measurement_temperature    149.8(4)
_cell_measurement_theta_max      70.3190
_cell_measurement_theta_min      4.1260
_cell_volume                     6767.61(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      149.8(4)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega   43.00   68.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 25

  2 omega  -11.00   30.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 41

  3 omega  -18.00    8.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -90.0000 26

  4 omega  -81.00  -47.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000    0.0000 34

  5 omega  -75.00  -37.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000   90.0000 38

  6 omega   37.00   88.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000   60.0000 51

  7 omega   33.00  118.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000  -90.0000 85

  8 omega   57.00   83.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -135.0000  104.0000 26

  9 omega  -15.00   79.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000  -60.0000 94

 10 omega   54.00   95.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -91.0000 -150.0000 41

 11 omega   74.00  114.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000    0.0000 40

 12 omega  153.00  178.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000 -180.0000 25

 13 omega   39.00   93.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -38.0000  -60.0000 54

 14 omega  107.00  142.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -91.0000 -150.0000 35

 15 omega   41.00   92.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -38.0000 -150.0000 51

 16 omega   50.00   83.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -38.0000  150.0000 33

 17 omega   41.00   67.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000    0.0000 26

 18 omega   49.00  139.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   12.0000 -150.0000 90
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0655880000
_diffrn_orient_matrix_UB_12      -0.0697334000
_diffrn_orient_matrix_UB_13      0.0103119000
_diffrn_orient_matrix_UB_21      0.0603118000
_diffrn_orient_matrix_UB_22      -0.0756672000
_diffrn_orient_matrix_UB_23      0.0112819000
_diffrn_orient_matrix_UB_31      -0.0000847000
_diffrn_orient_matrix_UB_32      0.0287672000
_diffrn_orient_matrix_UB_33      0.0546518000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17913
_diffrn_reflns_theta_full        70.68
_diffrn_reflns_theta_max         70.68
_diffrn_reflns_theta_min         4.14
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.816
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.00021(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         6415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0728P)^2^+3.0117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1209
_reflns_number_gt                5856
_reflns_number_total             6415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502685f_si_002.cif
_cod_data_source_block           xiongjiao0604
_cod_depositor_comments
'Adding full bibliography for 4342282--4342283.cif.'
_cod_original_cell_volume        6767.62(19)
_cod_database_code               4342283
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C35(H35A,
 H35B), C38(H38A,H38B), C39(H39A,H39B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C13(H13), C14(H14), C15(H15),
 C16(H16), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25)
;
_olex2_submission_special_instructions 'No special instructions were received'