Highly Iso-Selective and Active Catalysts of Sodium and Potassium Monophenoxides Capped by a Crown Ether for the Ring-Opening Polymerization ofrac-Lactide
Zhang, Jinjin; Xiong, Jiao; Sun, Yangyang; Tang, Ning; Wu, Jincai; Macromolecules 47 (2014) 7789–; doi:10.1021/ma502000y

data_1518191
_publ_section_title
;
 Highly Iso-Selective and Active Catalysts of Sodium and Potassium
 Monophenoxides Capped by a Crown Ether for the Ring-Opening
 Polymerization ofrac-Lactide
;
_journal_issue                   22
_journal_name_full               Macromolecules
_journal_page_first              7789
_journal_paper_doi               10.1021/ma502000y
_journal_volume                  47
_journal_year                    2014
_chemical_formula_moiety         'C61 H89 K O8, 2(C7 H8)'
_chemical_formula_sum            'C75 H105 K O8'
_chemical_formula_weight         1173.68
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 116.816(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6270(6)
_cell_length_b                   20.5145(7)
_cell_length_c                   13.9260(6)
_cell_measurement_reflns_used    4226
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.2070
_cell_measurement_theta_min      3.6140
_cell_volume                     3474.4(3)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
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  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0135807000
_diffrn_orient_matrix_UB_12      0.0238768000
_diffrn_orient_matrix_UB_13      -0.0408855000
_diffrn_orient_matrix_UB_21      -0.0486809000
_diffrn_orient_matrix_UB_22      -0.0173935000
_diffrn_orient_matrix_UB_23      -0.0328444000
_diffrn_orient_matrix_UB_31      -0.0290686000
_diffrn_orient_matrix_UB_32      0.0179799000
_diffrn_orient_matrix_UB_33      0.0225063000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0828
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            18073
_diffrn_reflns_point_group_measured_fraction_full 0.869
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         2.992
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53957
_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 green'
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_description       block
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 2790 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         11847
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.0372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1418
_reflns_Friedel_coverage         0.686
_reflns_Friedel_fraction_full    0.733
_reflns_Friedel_fraction_max     0.726
_reflns_number_gt                8964
_reflns_number_total             11847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma502000y_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1518189--1518192.cif.'
_cod_original_cell_volume        3474.3(3)
_cod_database_code               1518191
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C11 H10 N O K'
_reflns_odcompleteness_completeness 99.77
_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. Others
 Fixed Sof: C12(0.6) H12A(0.6) H12B(0.6) H12C(0.6) C13(0.6) H13A(0.6)
 H13B(0.6) H13C(0.6) C14(0.6) H14A(0.6) H14B(0.6) H14C(0.6) C12'(0.4) H12D(0.4)
 H12E(0.4) H12F(0.4) C13'(0.4) H13D(0.4) H13E(0.4) H13F(0.4) C14'(0.4)
 H14D(0.4) H14E(0.4) H14F(0.4)
3.a Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,
 H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B),
 C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C19(H19), C21(H21), C33(H33), C35(H35), C49(H49), C48(H48),
 C47(H47), C46(H46), C45(H45), C68(H68), C67(H67), C66(H66), C65(H65), C64(H64),
  C75(H75), C74(H74), C73(H73), C72(H72), C71(H71)
3.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C29(H29A,H29B,
 H29C), C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C39(H39A,H39B,H39C), C38(H38A,
 H38B,H38C), C37(H37A,H37B,H37C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C12'(H12D,H12E,H12F), C13'(H13D,H13E,H13F),
 C14'(H14D,H14E,H14F), C62(H62A,H62B,H62C), C69(H69A,H69B,H69C)
;
_shelx_res_checksum              22989
_shelx_hkl_checksum              40583