Highly Active Chiral Zinc Catalysts for Immortal Polymerization of β-Butyrolactone Form Melt Processable Syndio-Rich Poly(hydroxybutyrate)
Ebrahimi, Tannaz; Aluthge, Dinesh C.; Hatzikiriakos, Savvas G.; Mehrkhodavandi, Parisa; Macromolecules  (2016) –; doi:10.1021/acs.macromol.6b01908

data_1544590
_publ_section_title
;
 Highly Active Chiral Zinc Catalysts for Immortal Polymerization of
 \b-Butyrolactone Form Melt Processable Syndio-Rich Poly(hydroxybutyrate)
;
_journal_name_full               Macromolecules
_journal_paper_doi               10.1021/acs.macromol.6b01908
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C82 H92 N4 O4 Si2 Zn2, C7 H8'
_chemical_formula_sum            'C89 H98 N4 O4 Si2 Zn2'
_chemical_formula_weight         1474.63
_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
_audit_creation_date             2016-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.820(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.894(2)
_cell_length_b                   33.799(7)
_cell_length_c                   21.937(5)
_cell_measurement_reflns_used    9764
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.684
_cell_measurement_theta_min      2.300
_cell_volume                     7906(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-DUO'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0751
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            128836
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.734
_diffrn_reflns_theta_min         1.533
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0891 before and 0.0700 after correction.
The Ratio of minimum to maximum transmission is 0.7731.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       blade
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.020(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1866
_refine_ls_number_reflns         36757
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0429P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.967
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                30969
_reflns_number_total             36757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma6b01908_si_002.cif
_cod_data_source_block           pm157_a
_cod_database_code               1544590
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.775
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.980(6) 0.020(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 N11(H11), N1(H1), N31(H31), C021(H021), C79(H79), C32(H32), C27(H27),
 C02M(H02M), N3(H3A), C78(H78), C1AA(H1AA), C04P(H04P)
3.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C31(H31A,H31B), C01H(H01A,H01B), C82(H82A,H82B), C02I(H02F,
 H02G), C02J(H02I,H02J), C80(H80A,H80B), C02Z(H02O,H02P), C75(H75A,H75B),
 C81(H81A,H81B), C03U(H03A,H03B), C042(H04A,H04B), C28(H28A,H28B), C04F(H04D,
 H04E), C30(H30A,H30B), C29(H29A,H29B), C04Z(H04K,H04L), C058(H05A,H05B),
 C05C(H05D,H05E), C05F(H05F,H05G)
3.c Aromatic/amide H refined with riding coordinates:
 C11(H11A), C00T(H00T), C20(H20), C011(H011), C69(H69), C013(H013), C014(H014),
  C18(H18), C019(H019), C01E(H01E), C01G(H01G), C01I(H01I), C01K(H01K),
 C16(H16), C01M(H01M), C01N(H01N), C01O(H01O), C3(H3), C7(H7), C17(H17),
 C72(H72), C01W(H01W), C14(H14), C01Y(H01Y), C020(H020), C54(H54), C10(H10),
 C58(H58), C029(H029), C02A(H02A), C2(H2), C02C(H02C), C51(H51), C02H(H02H),
 C23(H23), C15(H15), C52(H52), C02W(H02W), C48(H48), C41(H41), C035(H035),
 C44(H44), C039(H039), C4(H4), C60(H60), C03D(H03H), C37(H37), C8(H8),
 C03H(H03I), C59(H59), C56(H56), C50(H50), C03M(H03M), C03O(H03O), C6(H6),
 C57(H57), C40(H40), C03X(H03X), C03Y(H03Y), C66(H66), C041(H041), C65(H65),
 C9(H9), C53(H53), C64(H64), C049(H049), C5(H5), C04B(H04C), C38(H38),
 C04G(H04G), C04H(H04H), C04I(H04M), C62(H62), C04N(H04N), C04O(H04O), C47(H47),
  C04S(H04S), C39(H39), C45(H45), C04W(H04W), C04Y(H04Y), C051(H051),
 C052(H052), C053(H053), C46(H46), C056(H056), C057(H057), C059(H059),
 C05A(H05Q), C05B(H05C), C63(H63), C05E(H05K), C05H(H05R), C05I(H05S),
 C05K(H05L), C05L(H05T), C05N(H05P), C05P(H05X)
3.d Idealised Me refined as rotating group:
 C71(H71A,H71B,H71C), C77(H77A,H77B,H77C), C02D(H02B,H02D,H02E), C33(H33A,H33B,
 H33C), C22(H22A,H22B,H22C), C02Y(H02K,H02L,H02N), C037(H03C,H03D,H03E),
 C34(H34A,H34B,H34C), C03Q(H03J,H03K,H03L), C76(H76A,H76B,H76C), C04X(H04F,H04I,
 H04J), C05G(H05H,H05I,H05J), C05M(H05M,H05N,H05O), C05O(H05U,H05V,H05W)
;
_shelx_res_checksum              41992
_shelx_hkl_checksum              81709
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'