Post-Synthetically Elaborated BODIPY-based Porous Organic Polymers (POPs) for Photochemical Detoxification of a Sulfur Mustard Simulant.
Atilgan, Ahmet; Cetin, M. Mustafa; Yu, Jierui; Beldjoudi, Yassine; Liu, Jian; Stern, Charlotte L.; Cetin, Furkan M.; Islamoglu, Timur; Farha, Omar K.; Deria, Pravas; Stoddart, J. Fraser; Hupp, Joseph T.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c07784

data_4135308
_publ_section_title
;
 Post-Synthetically Elaborated BODIPY-based Porous Organic Polymers (POPs)
 for Photochemical Detoxification of a Sulfur Mustard Simulant.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c07784
_journal_year                    2020
_chemical_formula_moiety         'C35 H24 B Br5 N2, C3 H7 N O'
_chemical_formula_sum            'C38 H31 B Br5 N3 O'
_chemical_formula_weight         956.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.472(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.388(2)
_cell_length_b                   24.134(3)
_cell_length_c                   9.6240(11)
_cell_measurement_reflns_used    6023
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.011
_cell_measurement_theta_min      3.358
_cell_volume                     3646.1(8)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2017)'
_computing_data_collection       'APEX2 V2017.3 (Bruker, 2017)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.93
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8809
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        65.024
_diffrn_reflns_theta_max         65.024
_diffrn_reflns_theta_min         3.358
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    6.945
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0828 before and 0.0388 after correction. The Ratio of minimum to maximum transmission is 0.8119. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1872
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3073
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+9.8533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2916
_reflns_number_total             3073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c07784_si_004.cif
_cod_data_source_block           cx1491
_cod_original_cell_volume        3646.0(8)
_cod_database_code               4135308
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.759
_shelx_estimated_absorpt_t_min   0.281
_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. Restrained distances
 O1S-C1S
 1.2 with sigma of 0.02
 N1S-C2S \\sim N1S-C1S \\sim N1S-C3S
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Br3A \\sim Br3: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Rigid body (RIGU) restrains
 O1S, N1S, C1S, C2S, C3S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Br3A)=0.5*(1-FVAR(2))
 Sof(Br3)=0.5*FVAR(2)
 Fixed Sof: O1S(0.5) N1S(0.5) C1S(0.5) H1S(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5)
 H2SC(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) H3SC(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C14(H14), C15(H15), C17(H17), C18(H18), C1S(H1S)
6.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C20(H20A,H20B,H20C), C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC)
;
_shelx_res_checksum              48384
_shelx_hkl_checksum              75082
_olex2_date_sample_data_collection 2019-01-24
_olex2_date_sample_submission    2019-01-23
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder'
_olex2_submission_original_sample_id cx1491
_olex2_submission_special_instructions 'No special instructions were received'