CO2-Involved and Isocyanide-Based Three-Component Polymerization toward Functional Heterocyclic Polymers with Self-Assembly and Sensing Properties
Liu, Dongming; Song, Bo; Wang, Jia; Li, Baoxi; Wang, Bingnan; Li, Mingzhao; Qin, Anjun; Tang, Ben Zhong; Macromolecules  (2021) –; doi:10.1021/acs.macromol.1c00312

data_1561944
_publ_section_title
;
 CO2-Involved and Isocyanide-Based Three-Component Polymerization toward
 Functional Heterocyclic Polymers with Self-Assembly and Sensing
 Properties
;
_journal_name_full               Macromolecules
_journal_paper_doi               10.1021/acs.macromol.1c00312
_journal_year                    2021
_chemical_formula_moiety         '2(C38 H36 N4 O4), 3(C4 H8 O)'
_chemical_formula_sum            'C88 H96 N8 O11'
_chemical_formula_weight         1441.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.6420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.1177(8)
_cell_length_b                   5.9556(2)
_cell_length_c                   29.0641(9)
_cell_measurement_reflns_used    9176
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.80
_cell_volume                     4102.8(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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'zju Bruker D8 Venture Ims3.0'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            43035
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.244
_diffrn_reflns_theta_min         2.427
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1624 before and 0.0588 after correction.
The Ratio of minimum to maximum transmission is 0.9348.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_description       needle
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         9126
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0742
_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^)+(0.1321P)^2^+2.3576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2096
_refine_ls_wR_factor_ref         0.2314
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6651
_reflns_number_total             9126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma1c00312_si_002.cif
_cod_data_source_block           191204_ldm352_0m
_cod_database_code               1561944
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.972
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O5-C39 \\sim C40A-C39 \\sim C40-C39 \\sim C41A-C40A \\sim C41-C40 \\sim
C42-C41 \\sim C42-C41A \\sim O5-C42
 with sigma of 0.02
 C19-C20 \\sim C19-C20A
 with sigma of 0.02
 C19-C21 \\sim C19-C21A
 with sigma of 0.02
 C19-C22 \\sim C19-C22A
 with sigma of 0.02
3. Rigid bond restraints
 C25, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C19, C20, C21, C22, C20A, C21A, C22A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C39 \\sim C40 \\sim C41 \\sim C40A \\sim C41A: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02
C19 \\sim C20 \\sim C21 \\sim C22 \\sim C20A \\sim C21A \\sim C22A: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(H39C)=Sof(H39D)=Sof(H42C)=Sof(H42D)=Sof(C40A)=Sof(H40D)=Sof(H40C)=
 Sof(C41A)=Sof(H41D)=Sof(H41C)=1-FVAR(1)
 Sof(H39A)=Sof(H39B)=Sof(H42A)=Sof(H42B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=
 Sof(H41A)=Sof(H41B)=FVAR(1)
 Sof(C20A)=Sof(H20F)=Sof(H20D)=Sof(H20E)=Sof(C21A)=Sof(H21D)=Sof(H21E)=
 Sof(H21F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(2)
 Sof(C20)=Sof(H20A)=Sof(H20C)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(2)
 Fixed Sof: O6(0.5) C43(0.5) H43A(0.5) H43B(0.5) C44(0.5) H44A(0.5) H44B(0.5)
 C45(0.5) H45A(0.5) H45B(0.5) C46(0.5) H46A(0.5) H46B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C39(H39C,H39D), C42(H42A,H42B), C42(H42C,H42D), C40(H40A,
 H40B), C41(H41A,H41B), C40A(H40D,H40C), C41A(H41D,H41C), C43(H43A,H43B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4), C5(H5), C6(H6), C8(H8), C12(H12), C13(H13), C16(H16),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
  C33(H33), C34(H34)
6.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C20(H20A,H20C,
 H20B), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C20A(H20F,H20D,H20E),
 C21A(H21D,H21E,H21F), C22A(H22D,H22E,H22F)
;
_shelx_res_checksum              43461
_shelx_hkl_checksum              4258
_olex2_submission_special_instructions 'No special instructions were received'