Multicomponent polymerization: development of a one-pot synthetic route to functional polymers using diyne, N-sulfonyl azide and water/ethanol as reactants
Deng, Haiqin; Han, Ting; Zhao, Engui; Kwok, Ryan T. K.; Lam, Jacky W. Y.; Tang, Ben Zhong; Polym. Chem. 7 (2016) 5646–; doi:10.1039/C6PY01337F

data_1543988
_publ_section_title
;
 Multicomponent polymerization: development of a one-pot synthetic route
 to functional polymers using diyne, N-sulfonyl azide and water/ethanol as
 reactants
;
_journal_issue                   36
_journal_name_full               'Polym. Chem.'
_journal_page_first              5646
_journal_paper_doi               10.1039/C6PY01337F
_journal_volume                  7
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C35 H29 N O3 S, C H2 Cl2'
_chemical_formula_sum            'C36 H31 Cl2 N O3 S'
_chemical_formula_weight         628.58
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_audit_update_record
;
2016-01-14 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   128.559(3)
_cell_length_b                   18.5908(4)
_cell_length_c                   5.29842(10)
_cell_measurement_reflns_used    5454
_cell_measurement_temperature    99.9(6)
_cell_measurement_theta_max      74.4630
_cell_measurement_theta_min      4.7910
_cell_volume                     12663.3(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3587
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
  1 omega   76.00  178.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.7843   77.0000 -180.0000 204

  2 omega  -41.00   70.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4812  -37.0000   60.0000 222

  3 omega    7.00  118.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4812   37.0000    0.0000 222

  4 omega   31.00   90.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.7843  -30.0000   60.0000 118

  5 omega   34.00   98.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.7843  -45.0000   30.0000 128

  6 omega  100.00  178.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.7843  111.0000   90.0000 156

  7 omega   31.00   90.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.7843  -30.0000 -150.0000 118

  8 omega   30.00  116.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.7843 -111.0000   30.0000 172

  9 omega -124.00  -79.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.4812  -99.0000   90.0000 90

 10 omega -123.00   -2.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.4812  -77.0000  150.0000 242

 11 omega   79.00   95.50   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.7843   61.0000    0.0000 33
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0115681000
_diffrn_orient_matrix_UB_12      -0.0131942000
_diffrn_orient_matrix_UB_13      -0.0602071000
_diffrn_orient_matrix_UB_21      0.0002821000
_diffrn_orient_matrix_UB_22      0.0610958000
_diffrn_orient_matrix_UB_23      -0.1965363000
_diffrn_orient_matrix_UB_31      0.0031188000
_diffrn_orient_matrix_UB_32      -0.0544040000
_diffrn_orient_matrix_UB_33      -0.2056353000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_limit_h_max       140
_diffrn_reflns_limit_h_min       -154
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            12221
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.46
_diffrn_reflns_theta_min         4.81
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.753
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5248
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.029(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         4619
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+38.4860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.0986
_reflns_number_gt                4360
_reflns_number_total             4619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6py01337f2.cif
_cod_data_source_block           TPE-amide
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 

 Adding full bibliography for 1543988--1543989.cif.
;
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               1543988
_reflns_odcompleteness_completeness 99.76
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1-C1S \\sim Cl2-C1S \\sim Cl2A-C1SA \\sim Cl1-C1SA
 with sigma of 0.02
3. Others
 Fixed Sof: C1S(0.8) C1SA(0.2) Cl2(0.8) Cl2A(0.2)
4.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C1S(H1SA,H1SB)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C15(H15),
 C16(H16), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C33(H33),
  C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_olex2_submission_special_instructions 'No special instructions were received'