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_4515185
_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         'C31 H22 N2 O4 S'
_chemical_formula_sum            'C31 H22 N2 O4 S'
_chemical_formula_weight         518.56
_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             2018-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.193(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0655(2)
_cell_length_b                   10.1856(3)
_cell_length_c                   27.0162(7)
_cell_measurement_reflns_used    7682
_cell_measurement_temperature    107(5)
_cell_measurement_theta_max      73.4300
_cell_measurement_theta_min      3.2780
_cell_volume                     2494.07(11)
_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      107(5)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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    -86.00 -52.00   0.50    0.50    --    0.00 -38.00  60.00   68
  2  \w    -14.00  44.00   0.50    0.50    --    0.00  19.00  60.00  116
  3  \w    -34.00   1.00   0.50    0.50    --    0.00 -38.00  60.00   70
  4  \w    -28.00   8.00   0.50    0.50    --    5.00 -57.00 -90.00   72
  5  \w    -81.00 -44.00   0.50    0.50    --    5.00 -57.00 -90.00   74
  6  \w   -117.00 -89.00   0.50    0.50    --  -98.80 -72.00 -90.00   56
  7  \w   -185.00-130.00   0.50    0.50    --  -98.80 -72.00 -90.00  110
  8  \w   -187.00-105.00   0.50    0.50    --  -98.80 -72.00 -30.00  164
  9  \w   -106.00 -34.00   0.50    0.50    --  -98.80  19.00 -90.00  144
 10  \w   -111.00 -12.00   0.50    0.50    --  -98.80  57.00  90.00  198
 11  \w   -112.00 -20.00   0.50    0.50    --  -98.80  38.00 -90.00  184
 12  \w   -102.00 -34.00   0.50    0.50    --  -98.80  19.00  60.00  136
 13  \w   -119.00 -94.00   0.50    0.50    --  -98.80 -52.00 136.00   50
 14  \w   -106.00 -96.50   0.50    0.50    --  -98.80  38.00  60.00   19
;
_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      -0.0543059000
_diffrn_orient_matrix_UB_12      0.1171697000
_diffrn_orient_matrix_UB_13      -0.0313625000
_diffrn_orient_matrix_UB_21      0.1582602000
_diffrn_orient_matrix_UB_22      0.0232352000
_diffrn_orient_matrix_UB_23      -0.0175922000
_diffrn_orient_matrix_UB_31      -0.0290912000
_diffrn_orient_matrix_UB_32      -0.0929170000
_diffrn_orient_matrix_UB_33      -0.0442947000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            10436
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.051
_diffrn_reflns_theta_max         67.051
_diffrn_reflns_theta_min         3.272
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.497
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82122
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0664P)^2^+3.6622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1574
_refine_ls_wR_factor_ref         0.1594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4030
_reflns_number_total             4372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mz9b00297_si_003.cif
_cod_data_source_block           3
_cod_database_code               4515185
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.865
_reflns_odcompleteness_completeness 98.12
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00V(H00A,H00C)
2.b Aromatic/amide H refined with riding coordinates:
 C008(H008), C00B(H00B), C00E(H00E), C00G(H00G), C00H(H00H), C00L(H00L),
 C00M(H00M), C00N(H00N), C00O(H00O), C00Q(H00Q), C00R(H00R), C00S(H00S),
 C00U(H00U), C00X(H00X), C00Y(H00Y), C010(H010), C011(H011)
2.c Idealised Me refined as rotating group:
 C012(H01A,H01B,H01C)
;
_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 1.304
_oxdiff_exptl_absorpt_empirical_full_min 0.777