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_4135307
_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 Br3 I2 N2, C3 H7 N O'
_chemical_formula_sum            'C38 H31 B Br3 I2 N3 O'
_chemical_formula_weight         1050.00
_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                 112.936(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.398(3)
_cell_length_b                   23.989(4)
_cell_length_c                   9.6741(12)
_cell_measurement_reflns_used    2188
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.060
_cell_measurement_theta_min      3.317
_cell_volume                     3718.4(10)
_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    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.93
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6222
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        63.680
_diffrn_reflns_theta_max         63.680
_diffrn_reflns_theta_min         3.317
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    17.330
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.4559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1046 before and 0.0588 after correction. The Ratio of minimum to maximum transmission is 0.6058. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_description       plate
_exptl_crystal_F_000             2016
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         2965
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0764P)^2^+33.7391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2408
_reflns_number_total             2965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c07784_si_005.cif
_cod_data_source_block           cx1492
_cod_database_code               4135307
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.140
_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. Rigid body (RIGU) restrains
 O, N1S, C1S, C2S, C3S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed Sof: O(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)
4.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C14(H14), C15(H15), C17(H17), C18(H18), C1S(H1S)
4.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              43158
_shelx_hkl_checksum              66942
_olex2_date_sample_data_collection 2019-01-25
_olex2_date_sample_submission    2019-01-25
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder'
_olex2_submission_original_sample_id cx1492
_olex2_submission_special_instructions 'No special instructions were received'