Benzyne–azide polycycloaddition: a facile route toward functional polybenzotriazoles
Xin, Dehua; Qin, Anjun; Tang, Ben Zhong; Polymer Chemistry 10 (2019) 4271–; doi:10.1039/C9PY00632J

data_1551823
_publ_section_title
;
 Benzyne--azide polycycloaddition: a facile route toward functional
 polybenzotriazoles
;
_journal_issue                   31
_journal_name_full               'Polymer Chemistry'
_journal_page_first              4271
_journal_paper_doi               10.1039/C9PY00632J
_journal_volume                  10
_journal_year                    2019
_chemical_formula_moiety         'C34 H34 F6 O6 S2 Si2'
_chemical_formula_sum            'C34 H34 F6 O6 S2 Si2'
_chemical_formula_weight         772.91
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-15 deposited with the CCDC.    2019-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.7450(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6890(2)
_cell_length_b                   9.29070(10)
_cell_length_c                   20.9995(2)
_cell_measurement_reflns_used    10441
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      73.3410
_cell_measurement_theta_min      4.1970
_cell_volume                     3638.44(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_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      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -88.00   2.00   0.50    0.50    --    0.00 -57.00 120.00  180
  2  \w    -82.00 -57.00   0.50    0.50    --    0.00 -57.00-150.00   50
  3  \w    -25.00  13.00   0.50    0.50    --    0.00 -19.00-150.00   76
  4  \w    -88.00 -62.00   0.50    0.50    --    0.00 -19.00-150.00   52
  5  \w    -56.00   2.00   0.50    0.50    --    0.00 -57.00-150.00  116
  6  \w   -105.00 -15.00   0.50    0.71    --  -98.80  38.00-180.00  180
  7  \w    -58.00  -9.00   0.50    0.71    --  -98.80  57.00 -60.00   98
  8  \w    -39.00 -13.00   0.50    0.71    --  -98.80  72.00 -30.00   52
  9  \w   -109.00 -17.00   0.50    0.71    --  -98.80  38.00 -60.00  184
 10  \w   -107.00 -31.00   0.50    0.71    --  -98.80  19.00 -60.00  152
 11  \w   -111.00 -61.00   0.50    0.71    --  -98.80  72.00 -30.00  100
 12  \w   -184.00 -94.00   0.50    0.71    --  -98.80 -72.00-180.00  180
 13  \w   -104.00 -78.00   0.50    0.71    --  -98.80  57.00 -60.00   52
 14  \w   -110.00 -24.00   0.50    0.71    --  -98.80  19.00-180.00  172
;
_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      0.0013826000
_diffrn_orient_matrix_UB_12      0.0298241000
_diffrn_orient_matrix_UB_13      -0.0720268000
_diffrn_orient_matrix_UB_21      -0.0412189000
_diffrn_orient_matrix_UB_22      0.1414180000
_diffrn_orient_matrix_UB_23      0.0083688000
_diffrn_orient_matrix_UB_31      0.0716243000
_diffrn_orient_matrix_UB_32      0.0813861000
_diffrn_orient_matrix_UB_33      0.0117747000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17802
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         2.369
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    2.613
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         6479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0436P)^2^+2.6860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.0990
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5861
_reflns_number_total             6479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9py00632j2.cif
_cod_data_source_block           xdh_2
_cod_depositor_comments          'Adding full bibliography for 1551823.cif.'
_cod_database_code               1551823
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.859
_shelx_estimated_absorpt_t_min   0.818
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00M(H00M), C00P(H00P), C00S(H00S), C00T(H00T), C00U(H00U), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010), C013(H013), C014(H014),
 C016(H016), C01B(H01P), C01C(H01Q), C01D(H01R)
2.b Idealised Me refined as rotating group:
 C011(H01A,H01B,H01C), C012(H01D,H01E,H01F), C015(H01G,H01H,H01I), C019(H01J,
 H01K,H01L), C01A(H01M,H01N,H01O), C01E(H01S,H01T,H01U)
;
_shelx_res_checksum              78683
_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 1.222
_oxdiff_exptl_absorpt_empirical_full_min 0.791