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_1544591
_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         'C29 H43.04 N3 O2 Zn'
_chemical_formula_sum            'C29 H45 N3 O2 Zn'
_chemical_formula_weight         533.05
_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   mixed
_audit_creation_date             2016-07-04
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.724(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1804(11)
_cell_length_b                   13.0247(13)
_cell_length_c                   19.4626(19)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    90
_cell_measurement_theta_max      28.54
_cell_measurement_theta_min      2.41
_cell_volume                     2820.0(5)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      90
_diffrn_detector                 'Bruker APEX2 area detector'
_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 0.997
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker D8 diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53818
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.575
_diffrn_reflns_theta_min         1.831
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0554 before and 0.0417 after correction.
The Ratio of minimum to maximum transmission is 0.8381.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       RECTANGULAR
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.401
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         7170
_refine_ls_number_restraints     390
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0383P)^2^+6.3256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1369
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6084
_reflns_number_total             7170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma6b01908_si_002.cif
_cod_data_source_block           pm173_p21onc
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               1544591
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.714
_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. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(C16A)=
 Sof(H16A)=Sof(C21A)=Sof(H21A)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C18A)=
 Sof(H18C)=Sof(H18D)=Sof(N2A)=Sof(Zn2)=1-FVAR(1)
 Sof(Zn1)=Sof(N2)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H15A)=Sof(H15B)=Sof(C16)=
 Sof(H16)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C21)=Sof(H21)=Sof(C19)=Sof(H19C)=
 Sof(H19D)=Sof(C17)=Sof(H17C)=Sof(H17D)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C16(H16), C21(H21), C16A(H16A), C21A(H21A)
4.b Secondary CH2 refined with riding coordinates:
 C17A(H17A,H17B), C20(H20A,H20B), C15(H15A,H15B), C18(H18A,H18B), C19A(H19A,
 H19B), C20A(H20C,H20D), C19(H19C,H19D), C18A(H18C,H18D), C17(H17C,H17D)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C29(H29), C14(H14), C28(H28), C26(H26), C27(H27)
4.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C4(H4A,H4B,H4C),
 C23(H23A,H23B,H23C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C22(H22A,H22B,H22C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'