Preparation and Characterization of a Small Library of Thermally-Labile End-Caps for Variable-Temperature Triggering of Self-Immolative Polymers.
Taimoory, S. Maryamdokht; Sadraei, S. Iraj; Fayoumi, Rose Anne; Nasri, Sarah; Revington, Matthew; Trant, John F.; The Journal of organic chemistry 83 (2018) 4427–4440; doi:10.1021/acs.joc.8b00135

data_4034950
_publ_section_title
;
 Preparation and Characterization of a Small Library of Thermally-Labile
 End-Caps for Variable-Temperature Triggering of Self-Immolative Polymers.
;
_journal_issue                   8
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              4427
_journal_page_last               4440
_journal_paper_doi               10.1021/acs.joc.8b00135
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C16 H14 N2 O6'
_chemical_formula_sum            'C16 H14 N2 O6'
_chemical_formula_weight         330.29
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.621(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.002(4)
_cell_length_b                   6.3616(11)
_cell_length_c                   13.302(3)
_cell_measurement_reflns_used    9662
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.336
_cell_measurement_theta_min      3.069
_cell_volume                     1435.9(5)
_computing_cell_refinement       'Bruker APEX-II'
_computing_data_collection       'Bruker APEX-II'
_computing_data_reduction        'Bruker APEX-II'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II with Photon 100 CCD detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36940
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.474
_diffrn_reflns_theta_min         3.069
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
sadabs 2016/2 Bruker AXS Madison WI USA
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       plate
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_parameters     221
_refine_ls_number_reflns         2952
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0425P)^2^+1.1983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2346
_reflns_number_total             2952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b00135_si_001.cif
_cod_data_source_block           HENT_22_2bis_a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4034950
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              35599
_shelx_hkl_checksum              74802