Direct Construction of Acid-Responsive Poly(indolone)s through Multicomponent Tandem Polymerizations
Qi, Chunxuan; Zheng, Chao; Hu, Rongrong; Tang, Ben Zhong; ACS Macro Letters  (2019) 569–; doi:10.1021/acsmacrolett.9b00297

data_4515186
_publ_section_title
;
 Direct Construction of Acid-Responsive Poly(indolone)s through
 Multicomponent Tandem Polymerizations
;
_journal_name_full               'ACS Macro Letters'
_journal_page_first              569
_journal_paper_doi               10.1021/acsmacrolett.9b00297
_journal_year                    2019
_chemical_formula_moiety         'C35 H31 N3 O3 S'
_chemical_formula_sum            'C35 H31 N3 O3 S'
_chemical_formula_weight         573.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                99.466(2)
_cell_angle_beta                 111.743(2)
_cell_angle_gamma                99.2606(19)
_cell_formula_units_Z            2
_cell_length_a                   10.38019(19)
_cell_length_b                   11.4130(3)
_cell_length_c                   13.9290(3)
_cell_measurement_reflns_used    8009
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      73.4530
_cell_measurement_theta_min      3.5670
_cell_volume                     1466.89(6)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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    -89.00 -59.00   0.50    0.50    --    0.00 -72.00  90.00   60
  2  \w    -86.00 -35.00   0.50    0.50    --    0.00 -72.00 -60.00  102
  3  \w    -52.00  11.00   0.50    0.50    --    0.00 -72.00  90.00  126
  4  \w    -29.00   4.00   0.50    0.50    --    0.00 -72.00 -60.00   66
  5  \w    -89.00 -11.00   0.50    0.50    --    0.00 -19.00 150.00  156
  6  \w     54.00  92.00   0.50    0.50    --    5.00  72.00 -60.00   76
  7  \w     -1.00  24.00   0.50    0.50    --    5.00  72.00 -60.00   50
  8  \w   -108.00 -17.00   0.50    0.50    --  -98.80  72.00 -60.00  182
  9  \w   -110.00 -21.00   0.50    0.50    --  -98.80  19.00-150.00  178
 10  \w    -95.00 -52.00   0.50    0.50    --  -98.80  72.00  30.00   86
 11  \w   -113.00 -51.00   0.50    0.50    --  -98.80  72.00 150.00  124
 12  \w   -109.00 -80.00   0.50    0.50    --  -98.80  72.00   0.00   58
 13  \w    -75.00 -24.00   0.50    0.50    --  -98.80  72.00   0.00  102
 14  \w    -95.00 -40.00   0.50    0.50    --  -98.80  72.00-180.00  110
 15  \w   -104.00 -15.00   0.50    0.50    --  -98.80  19.00  90.00  178
 16  \w   -102.00 -28.00   0.50    0.50    --  -98.80  72.00  90.00  148
 17  \w    -50.00 -11.00   0.50    0.50    --  -98.80  19.00 -60.00   78
 18  \w    -50.00 -13.00   0.50    0.50    --  -98.80  57.00 -60.00   74
 19  \w   -113.00 -54.00   0.50    0.50    --  -98.80  57.00 -60.00  118
 20  \w    -42.00 -17.00   0.50    0.50    --  -98.80  72.00 120.00   50
 21  \w    -88.00 -63.00   0.50    0.50    --  -98.80  72.00 120.00   50
 22  \w    -45.00 -20.00   0.50    0.50    --  -98.80  72.00  30.00   50
 23  \w   -105.00 -19.00   0.50    0.50    --  -98.80  72.00-150.00  172
 24  \w   -105.00 -80.00   0.50    0.50    --  -98.80  72.00 -90.00   50
 25  \w   -183.00 -10.00   0.50    0.50    --  -98.80   0.00  60.00  346
;
_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      0.0634849000
_diffrn_orient_matrix_UB_12      0.0401179000
_diffrn_orient_matrix_UB_13      0.1226329000
_diffrn_orient_matrix_UB_21      -0.0242364000
_diffrn_orient_matrix_UB_22      -0.1352110000
_diffrn_orient_matrix_UB_23      0.0050388000
_diffrn_orient_matrix_UB_31      0.1500087000
_diffrn_orient_matrix_UB_32      -0.0013311000
_diffrn_orient_matrix_UB_33      0.0038780000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12730
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.040
_diffrn_reflns_theta_max         67.040
_diffrn_reflns_theta_min         3.523
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.305
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90031
_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_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         5148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0397P)^2^+0.5593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0940
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4671
_reflns_number_total             5148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mz9b00297_si_002.cif
_cod_data_source_block           qcx_1
_cod_database_code               4515186
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.903
_reflns_odcompleteness_completeness 98.19
_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 C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N0) = Uanis(N008)
Uanis(C0) = Uanis(C014)
Uanis(C1) = Uanis(C015)
3. Others
 Sof(H00C)=Sof(H00D)=Sof(N0)=1-FVAR(1)
 Sof(N008)=Sof(H00A)=Sof(H00B)=FVAR(1)
 Sof(C0)=Sof(H0A)=Sof(H0B)=1-FVAR(2)
 Sof(C014)=Sof(H01D)=Sof(H01E)=FVAR(2)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=1-FVAR(3)
 Sof(C015)=Sof(H01F)=Sof(H01G)=Sof(H01H)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C00Z(H00A,H00B), C00Z(H00C,H00D), C014(H01D,H01E), C0(H0A,H0B)
4.b Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00G(H00G), C00H(H00H), C00I(H00I), C00J(H00J), C00K(H00K),
 C00M(H00M), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T),
 C00U(H00U), C00V(H00V), C00X(H00X), C010(H010), C011(H011), C012(H012)
4.c Idealised Me refined as rotating group:
 C013(H01A,H01B,H01C), C015(H01F,H01G,H01H), C016(H01I,H01J,H01K), C1(H1A,H1B,
 H1C)
;
_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 1.388
_oxdiff_exptl_absorpt_empirical_full_min 0.803