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_1544589
_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_formula_moiety         'C80 H100 N4 O4 Zn2'
_chemical_formula_sum            'C80 H100 N4 O4 Zn2'
_chemical_formula_weight         1312.37
_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
_audit_creation_date             2015-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                91.335(3)
_cell_angle_beta                 107.129(3)
_cell_angle_gamma                109.096(3)
_cell_formula_units_Z            1
_cell_length_a                   12.0439(15)
_cell_length_b                   12.0523(15)
_cell_length_c                   13.1052(16)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    90
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.44
_cell_volume                     1702.7(4)
_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, 2008)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48808
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.604
_diffrn_reflns_theta_min         1.640
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.758
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0562 before and 0.0501 after correction.
The Ratio of minimum to maximum transmission is 0.8437.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       blade
_exptl_crystal_F_000             700
_exptl_crystal_recrystallization_method
'grown in a mixture of dichloromethane and diethyl ether'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         10305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+0.6906P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0777
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8529
_reflns_number_total             10305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma6b01908_si_002.cif
_cod_data_source_block           pm149
_cod_database_code               1544589
_shelxl_version_number           2012-9
_olex2_refinement_description
;
1. 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
2.a Ternary CH refined with riding coordinates:
 N1(H1), C1(H1A), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B), C5(H5A,H5B), C9(H9A,H9B), C34(H34A,H34B)
2.c Aromatic/amide H refined with riding coordinates:
 C40(H40), C13(H13), C30(H30), C11(H11), C24(H24), C21(H21), C29(H29),
 C20(H20), C22(H22), C33(H33), C39(H39), C23(H23), C36(H36), C38(H38), C37(H37),
  C31(H31), C32(H32)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C7(H7A,H7B,H7C), C18(H18A,H18B,H18C),
 C27(H27A,H27B,H27C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              31247
_shelx_hkl_checksum              35580
_olex2_submission_special_instructions 'No special instructions were received'