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_1518192
_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         'C59 H85 Na O7, 0.5(C6.2 H6.2), C7 H8'
_chemical_formula_sum            'C69.1 H96.1 Na O7'
_chemical_formula_weight         1061.75
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 96.560(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.2485(7)
_cell_length_b                   30.3361(10)
_cell_length_c                   19.2625(5)
_cell_measurement_reflns_used    15825
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.6390
_cell_measurement_theta_min      4.0870
_cell_volume                     12915.8(7)
_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  'XH (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0501082000
_diffrn_orient_matrix_UB_12      -0.0305707000
_diffrn_orient_matrix_UB_13      -0.0343998000
_diffrn_orient_matrix_UB_21      0.0445222000
_diffrn_orient_matrix_UB_22      -0.0390816000
_diffrn_orient_matrix_UB_23      0.0068648000
_diffrn_orient_matrix_UB_31      -0.0191593000
_diffrn_orient_matrix_UB_32      -0.0108194000
_diffrn_orient_matrix_UB_33      0.0724401000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            73185
_diffrn_reflns_theta_full        66.00
_diffrn_reflns_theta_max         66.00
_diffrn_reflns_theta_min         3.72
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72199
_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 colourless'
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4622
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1514
_refine_ls_number_reflns         22234
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0725
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1268P)^2^+1.8374P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1955
_refine_ls_wR_factor_ref         0.2146
_reflns_number_gt                17138
_reflns_number_total             22234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ma502000y_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 1518189--1518192.cif.'
_cod_original_formula_sum        'C69.10 H96.10 Na O7'
_cod_database_code               1518192
_reflns_odcompleteness_completeness 93.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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. Restrained distances
 C14A-C14B
 1.54 with sigma of 0.02
 C14A-C15B = C14A-C19B
 2.54 with sigma of 0.02
3. Rigid bond restraints
 C14A, C14B, C15B, C16B, C17B, C18B, C19B, C14C
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C137, C138, C139, C134, C135, C136
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C14, C11, C12, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C14A \\sim C14B \\sim C15B \\sim C16B \\sim C17B \\sim C18B \\sim C19B \\sim
C14C: within 1.7A with sigma of 0.002 and sigma for terminal atoms of 0.008
C137 \\sim C138 \\sim C139 \\sim C134 \\sim C135 \\sim C136: within 1.7A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C14 \\sim C11 \\sim C12 \\sim C13: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
5. Others
 Sof(C12B)=Sof(H12G)=Sof(H12H)=Sof(H12I)=1-FVAR(1)
 Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=FVAR(1)
 Sof(C43')=Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(C42')=Sof(H42D)=Sof(H42E)=
 Sof(H42F)=Sof(C41')=Sof(H41D)=Sof(H41E)=Sof(H41F)=1-FVAR(2)
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(2)
 Fixed Sof: C14C(0.25) H14D(0.25) H14E(0.25) H14F(0.25) C14A(0.25) H14I(0.25)
 H14J(0.25) H14K(0.25) C14B(0.5) C15B(0.5) H15B(0.5) C16B(0.5) H16B(0.5)
 C17B(0.5) H17B(0.5) C18B(0.5) C19B(0.5) H19B(0.5) C134(0.45) H134(0.45)
 C135(0.45) H135(0.45) C136(0.45) H14G(0.45) C137(0.45) H14H(0.45) C138(0.45)
 H138(0.45) C139(0.45) H139(0.45)
6.a Secondary CH2 refined with riding coordinates:
 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), C110(H11A,H11B), C111(H11C,H11D), C112(H11E,H11F), C113(H11G,
 H11H), C114(H11I,H11J), C115(H11K,H11L), C116(H11M,H11N), C117(H11O,H11P),
 C118(H11Q,H11R), C119(H11S,H11T)
6.b Me refined with riding coordinates:
 C43'(H43D,H43E,H43F), C42'(H42D,H42E,H42F), C41'(H41D,H41E,H41F)
6.c Aromatic/amide H refined with riding coordinates:
 C15B(H15B), C16B(H16B), C17B(H17B), C19B(H19B), C3(H3), C5(H5), C19(H19),
 C21(H21), C33(H33), C35(H35), C63(H63), C65(H65), C79(H79), C81(H81), C93(H93),
  C95(H95), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C109(H109),
 C108(H108), C107(H107), C106(H106), C105(H105), C122(H122), C123(H123),
 C124(H124), C125(H125), C126(H126), C128(H128), C129(H129), C130(H130),
 C131(H131), C132(H132), C134(H134), C135(H135), C136(H14G), C137(H14H),
 C138(H138), C139(H139)
6.d Fitted hexagon refined as free rotating group:
 C14B(C15B,C16B,C17B,C18B,C19B), C134(C135,C136,C137,C138,C139)
6.e Idealised Me refined as rotating group:
 C14C(H14D,H14E,H14F), C14A(H14I,H14J,H14K), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C68(H68A,H68B,H68C), C69(H69A,H69B,
 H69C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C74(H74A,
 H74B,H74C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C),
 C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C97(H97A,H97B,
 H97C), C98(H98A,H98B,H98C), C99(H99A,H99B,H99C), C101(H10D,H10E,H10F),
 C102(H10G,H10H,H10I), C103(H10J,H10K,H10L), C120(H12J,H12K,H12L), C12A(H12D,
 H12E,H12F), C12B(H12G,H12H,H12I), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C),
 C42(H42A,H42B,H42C)
;
_shelx_hkl_checksum              11847