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_4134208
_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         '3(B F4), C48 H45 N6, O'
_chemical_formula_sum            'C48 H45 B3 F12 N6 O'
_chemical_formula_weight         982.33
_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             2019-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.674(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   57.282(7)
_cell_length_b                   11.7334(15)
_cell_length_c                   16.2714(18)
_cell_measurement_reflns_used    6701
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      44.923
_cell_measurement_theta_min      3.851
_cell_volume                     10580(2)
_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      101.93
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.381
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.381
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21998
_diffrn_reflns_point_group_measured_fraction_full 0.381
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         42.093
_diffrn_reflns_theta_min         3.851
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_T_max  0.7488
_exptl_absorpt_correction_T_min  0.5824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1242 before and 0.0637 after correction. The Ratio of minimum to maximum transmission is 0.7778. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       plate
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.738
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.324
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         3638
_refine_ls_number_restraints     374
_refine_ls_restrained_S_all      2.134
_refine_ls_R_factor_all          0.1973
_refine_ls_R_factor_gt           0.1698
_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          0.4544
_refine_ls_wR_factor_ref         0.4877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2408
_reflns_number_total             3638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13790_si_003.cif
_cod_data_source_block           Polymer
_cod_database_code               4134208
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.559
_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
 B2-F8
 1.4 with sigma of 0.02
 B4-F14 = B4-F13 = B4-F15 = B4-F16
 1.4 with sigma of 0.02
 C43-C44
 1.6 with sigma of 0.02
 H43-H40
 2 with sigma of 0.02
 H13A-H22B
 2 with sigma of 0.02
 H21C-H23B
 2 with sigma of 0.02
 B3-F11 \\sim B3-F12 \\sim B3-F9 \\sim B3-F10
 with sigma of 0.02
 F11-F12 \\sim F11-F9 \\sim F11-F10 \\sim F12-F9 \\sim F12-F10 \\sim F9-F10
 with sigma of 0.02
 F14-F13 \\sim F14-F15 \\sim F14-F16
 with sigma of 0.02
 F13-F15 \\sim F13-F16 \\sim F15-F16
 with sigma of 0.02
 F8-F5 \\sim F8-F6 \\sim F8-F7
 with sigma of 0.02
3. Restrained planarity
 C16, C15, C18, C14, C17, C19
 with sigma of 0.1
4. Rigid bond restraints
 F10, F11, B3, F9, F12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C3, C7, C6, N1, C4, C1, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F16, F14, F13, B4, F15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C47, C48, C44, C45, C46, N6, C43, C42, C39, C40, C41, C38, N5, C36, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
F10 \\sim F11 \\sim B3 \\sim F9 \\sim F12: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C2 \\sim C3 \\sim C7 \\sim C6 \\sim N1 \\sim C4 \\sim C1 \\sim C5: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
F5 \\sim F7 \\sim B2 \\sim F8 \\sim F6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
F16 \\sim F14 \\sim F13 \\sim B4 \\sim F15: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C47 \\sim C48 \\sim C44 \\sim C45 \\sim C46 \\sim N6 \\sim C43 \\sim C42 \\sim
C39 \\sim C40 \\sim C41 \\sim C38 \\sim N5 \\sim C36 \\sim C37: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C14 \\sim C15: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(B4) = Uanis(B3) = Uanis(B1) = Uanis(B2)
6. Others
 Fixed Sof: F7(0.5) F6(0.5) F5(0.5) F8(0.5) F14(0.5) F13(0.5) F15(0.5) F16(0.5)
7.a Ternary CH refined with riding coordinates:
 C7(H7), C6(H6), C43(H43), C42(H42)
7.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C13(H13A,H13B), C36(H36A,H36B)
7.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C2(H2), C29(H29), C32(H32), C24(H24), C10(H10), C25(H25), C35(H35),
 C12(H12), C27(H27), C28(H28), C11(H11), C33(H33), C34(H34), C9(H9), C4(H4),
 C41(H41), C40(H40), C38(H38), C37(H37), C1(H1), C5(H5), C47(H47), C48(H48),
 C45(H45), C46(H46)
7.d Fitted hexagon refined as free rotating group:
 N5(C41,C40,C39,C38,C37), C47(C48,C44,C45,C46,N6)
7.e Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
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_olex2_submission_special_instructions 'No special instructions were received'