Synthesis and characterization of BPA-free polyesters by incorporating a semi-rigid cyclobutanediol monomer
Shahni, Rahul K.; Mabin, Micah; Wang, Zhihan; Shaik, Muneer; Ugrinov, Angel; Chu, Qianli R.; Polymer Chemistry 11 (2020) 6081–6090; doi:10.1039/D0PY01098G

data_1558896
_publ_section_title
;
 Synthesis and characterization of BPA-free polyesters by incorporating a
 semi-rigid cyclobutanediol monomer
;
_journal_issue                   37
_journal_name_full               'Polymer Chemistry'
_journal_page_first              6081
_journal_page_last               6090
_journal_paper_doi               10.1039/D0PY01098G
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C18 H20 O2'
_chemical_formula_sum            'C18 H20 O2'
_chemical_formula_weight         268.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-24 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.9616(7)
_cell_length_b                   7.6761(3)
_cell_length_c                   21.5205(9)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      66.257
_cell_measurement_theta_min      4.109
_cell_volume                     2967.1(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      109.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0967
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            73145
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.885
_diffrn_reflns_theta_max         66.885
_diffrn_reflns_theta_min         4.108
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0992 before and 0.0634 after correction. The Ratio of minimum to maximum transmission is 0.8891. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       plate
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.2(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5263
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0782
_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^)+(0.1008P)^2^+4.5988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2040
_refine_ls_wR_factor_ref         0.2071
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4930
_reflns_number_total             5263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0py01098g2.cif
_cod_data_source_block           pna21
_cod_depositor_comments
;
Adding full bibliography for 1558896.cif.

2022-03-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C18 H20 O2)'
_cod_original_formula_sum        'C36 H40 O4'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     536.68
_cod_database_code               1558896
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.805
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8(6)
 0.2(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
3.a Ternary CH refined with riding coordinates:
 C009(H009), C00B(H00C), C00D(H00F), C00E(H00K), C00I(H00I), C00L(H00L),
 C00N(H00O), C00R(H00T)
3.b Secondary CH2 refined with riding coordinates:
 C006(H00A,H00B), C00C(H00D,H00E), C00M(H00M,H00N), C00P(H00R,H00S)
3.c Aromatic/amide H refined with riding coordinates:
 C007(H007), C008(H008), C00G(H00G), C00H(H00H), C00J(H00J), C00O(H00P),
 C00Q(H00Q), C00S(H00U), C00T(H00V), C00U(H00W), C00V(H00X), C00W(H00Y),
 C00X(H00), C00Y(H0AA), C00Z(H00Z), C010(H010), C011(H011), C012(H012),
 C013(H013), C014(H014)
3.d Idealised tetrahedral OH refined as rotating group:
 O001(H001), O002(H002), O003(H003), O004(H004)
;
_olex2_submission_special_instructions 'No special instructions were received'