Single-Crystal Polycationic Polymers Obtained by Single-Crystal-to-Single-Crystal Photopolymerization.
Guo, Qing-Hui; Jia, Manping; Liu, Zhichang; Qiu, Yunyan; Chen, Hongliang; Shen, Dengke; Zhang, Xuan; Tu, Qing; Ryder, Matthew R.; Chen, Haoyuan; Li, Peng; Xu, Yaobin; Li, Penghao; Chen, Zhijie; Shekhawat, Gajendra S.; Dravid, Vinayak P.; Snurr, Randall Q.; Philp, Douglas; Sue, Andrew C.-H.; Farha, Omar K.; Rolandi, Marco; Stoddart, J. Fraser; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b13790

data_4134207
_publ_section_title
;
 Single-Crystal Polycationic Polymers Obtained by
 Single-Crystal-to-Single-Crystal Photopolymerization.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b13790
_journal_year                    2020
_chemical_formula_moiety         '6(B F4), 3(O), 0.5(C192 H180 N24)'
_chemical_formula_sum            'C96 H90 B6 F24 N12 O3'
_chemical_formula_weight         1980.65
_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
_audit_creation_date             2019-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.731(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   57.8973(16)
_cell_length_b                   11.8809(3)
_cell_length_c                   15.7534(4)
_cell_measurement_reflns_used    6844
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      61.75
_cell_measurement_theta_min      3.14
_cell_volume                     10526.6(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.04
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.863
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.863
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       66
_diffrn_reflns_limit_h_min       -66
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19635
_diffrn_reflns_point_group_measured_fraction_full 0.863
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         62.402
_diffrn_reflns_theta_min         3.143
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  0.7522
_exptl_absorpt_correction_T_min  0.6287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0759 before and 0.0397 after correction. The Ratio of minimum to maximum transmission is 0.8358. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             4080
_exptl_crystal_size_max          0.394
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         8234
_refine_ls_number_restraints     443
_refine_ls_restrained_S_all      2.032
_refine_ls_R_factor_all          0.1650
_refine_ls_R_factor_gt           0.1469
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4258
_refine_ls_wR_factor_ref         0.4541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6164
_reflns_number_total             8234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13790_si_002.cif
_cod_data_source_block           Intermediate
_cod_database_code               4134207
_shelxl_version_number           2014/6
_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. Restrained distances
 F8-B3 = B2-F9 = B4-F16
 1.4 with sigma of 0.02
 B3-F7 \\sim B3-F5 \\sim B3-F8 \\sim B3-F6
 with sigma of 0.02
 B2-F9 \\sim B2-F10A \\sim B2-F12A \\sim B2-F11A
 with sigma of 0.02
 F9-F10A \\sim F9-F12A \\sim F9-F11A \\sim F10A-F12A \\sim F10A-F11A \\sim
F12A-F11A
 with sigma of 0.02
 B2-F12A \\sim B2-F11
 with sigma of 0.02
 B2-F11A \\sim B2-F10
 with sigma of 0.02
 B2-F10A \\sim B2-F12
 with sigma of 0.02
 B4-F16 \\sim B4-F13 \\sim B4-F14 \\sim B4-F15
 with sigma of 0.02
 F16-F13 \\sim F16-F14 \\sim F16-F15
 with sigma of 0.02
 F13-F14 \\sim F13-F15 \\sim F14-F15
 with sigma of 0.02
 F9-F10A \\sim F9-F12A \\sim F9-F11A \\sim F9-F10 \\sim F9-F12 \\sim F9-F11
 with sigma of 0.02
3. Rigid bond restraints
 N6, C44, C48, C47, C46, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F13, F14, F15, F16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F9, F10, F11, F12, F10A, F11A, F12A, B2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F14, F16, F13, F15, B4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C31, C32, C33, N4, C34, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N6 \\sim C44 \\sim C48 \\sim C47 \\sim C46 \\sim C45: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
F13 \\sim F14 \\sim F15 \\sim F16: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
F5 \\sim F6 \\sim F7 \\sim F8: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
F9 \\sim F10 \\sim F11 \\sim F12 \\sim F10A \\sim F11A \\sim F12A \\sim B2:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
F14 \\sim F16 \\sim F13 \\sim F15 \\sim B4: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
F8 \\sim F7 \\sim B3 \\sim F6 \\sim F5: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C43 \\sim C42: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
B4 \\sim B1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C31 \\sim C32 \\sim C33 \\sim N4 \\sim C34 \\sim C35: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(C44) \\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(B2) \\sim Ueq, Uanis(B4) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(F12A) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F13)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F16) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F16)
\\sim Ueq, Uanis(B4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(C29) = Uanis(C29A) = Uanis(C30A) = Uanis(C30)
5. Others
 Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=1-FVAR(1)
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=1-FVAR(2)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=FVAR(2)
 Fixed Sof: F5(0.5) F6(0.5) F7(0.5) F8(0.5) F13(0.5) F14(0.5) F15(0.5)
 F16(0.5) O2(0.5)
6.a Ternary CH refined with riding coordinates:
 C42(H42), C43(H43), C29A(H29A), C30A(H30A)
6.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C23(H23A,H23B), C36(H36A,H36B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11),
 C12(H12), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
  C33(H33), C34(H34), C40(H40), C41(H41), C37(H37), C38(H38), C48(H48),
 C47(H47), C46(H46), C45(H45), C35(H35)
6.d Fitted hexagon refined as free rotating group:
 C40(C41,N5,C37,C38,C39), C44(C48,C47,N6,C46,C45)
6.e Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_olex2_submission_special_instructions 'No special instructions were received'