Metal-free polycycloaddition of aldehyde-activated internal diynes and diazides toward post-functionalizable poly(formyl-1,2,3-triazole)s
Li, Baixue; Qin, Anjun; Tang, Ben Zhong; Polymer Chemistry 11 (2020) 3075–3083; doi:10.1039/D0PY00193G

data_1557775
_publ_section_title
;
 Metal-free polycycloaddition of aldehyde-activated internal diynes and
 diazides toward post-functionalizable poly(formyl-1,2,3-triazole)s
;
_journal_issue                   17
_journal_name_full               'Polymer Chemistry'
_journal_page_first              3075
_journal_page_last               3083
_journal_paper_doi               10.1039/D0PY00193G
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C16 H13 N3 O'
_chemical_formula_sum            'C16 H13 N3 O'
_chemical_formula_weight         263.29
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-12 deposited with the CCDC.	2020-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.249(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1254(7)
_cell_length_b                   8.1029(4)
_cell_length_c                   12.6860(7)
_cell_measurement_reflns_used    4567
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      73.3970
_cell_measurement_theta_min      6.5600
_cell_volume                     1273.78(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -62.00 -37.00   0.50    0.50    --    0.00 -56.00  44.00   50
  2  \w     18.00  43.00   0.50    0.50    --    5.00  56.00-173.00   50
  3  \w    -57.00 -32.00   0.50    0.50    --    5.00 -56.00  44.00   50
  4  \w   -141.00-116.00   0.50    0.50    --  -98.80 -56.00  44.00   50
  5  \w   -111.00 -60.00   0.50    0.50    --  -98.80  56.00-173.00  102
  6  \w    -41.00   9.00   0.50    0.50    --    0.00 -37.00 -30.00  100
  7  \w    -74.00 -47.00   0.50    0.50    --    0.00 -37.00 -30.00   54
  8  \w    -41.00   7.00   0.50    0.50    --    0.00 -72.00 150.00   96
  9  \w    -85.00 -45.00   0.50    0.50    --    0.00 -72.00 150.00   80
 10  \w   -110.00 -85.00   0.50    0.50    --  -98.80 -19.00-180.00   50
 11  \w    -96.00 -46.00   0.50    0.50    --  -98.80  37.00 -30.00  100
 12  \w   -102.00 -10.00   0.50    0.50    --  -98.80  37.00-180.00  184
 13  \w   -176.00-151.00   0.50    0.50    --  -98.80 -19.00 120.00   50
 14  \w   -186.00 -89.00   0.50    0.50    --  -98.80 -57.00  60.00  194
 15  \w   -141.00 -86.00   0.50    0.50    --  -98.80 -19.00 120.00  110
 16  \w   -103.00 -32.00   0.50    0.50    --  -98.80  37.00  30.00  142
 17  \w   -105.00 -15.00   0.50    0.50    --  -98.80  19.00   0.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0016346000
_diffrn_orient_matrix_UB_12      0.0550449000
_diffrn_orient_matrix_UB_13      -0.1154898000
_diffrn_orient_matrix_UB_21      -0.0951904000
_diffrn_orient_matrix_UB_22      -0.1156919000
_diffrn_orient_matrix_UB_23      -0.0561240000
_diffrn_orient_matrix_UB_31      -0.0797555000
_diffrn_orient_matrix_UB_32      0.1409888000
_diffrn_orient_matrix_UB_33      -0.0009064000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5898
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.567
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0610P)^2^+0.3595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1083
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2151
_reflns_number_total             2269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0py00193g2.cif
_cod_data_source_block           1
_cod_depositor_comments
;Adding full bibliography for 1557775--1557777.cif.

 Adding full bibliography for 1557775--1557777.cif.
;
_cod_original_cell_volume        1273.78(12)
_cod_database_code               1557775
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00C(H00C,H00D)
2.b Aromatic/amide H refined with riding coordinates:
 C009(H009), C00A(H00A), C00B(H00B), C00D(H00E), C00E(H00F), C00F(H00G),
 C00G(H00H), C00H(H00I), C00I(H00J), C00J(H00K), C00K(H00L)
;
_shelx_res_checksum              16681
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.335
_oxdiff_exptl_absorpt_empirical_full_min 0.659