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_4134206
_publ_section_title
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 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), 1.33(H2 O), C48 H45 N6'
_chemical_formula_sum            'C48 H47.67 B3 F12 N6 O1.33'
_chemical_formula_weight         990.35
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.308(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   58.143(2)
_cell_length_b                   11.9245(5)
_cell_length_c                   15.4738(7)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.43
_cell_measurement_theta_min      3.11
_cell_volume                     10481.8(7)
_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      100.02
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       67
_diffrn_reflns_limit_h_min       -67
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23102
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        65.635
_diffrn_reflns_theta_max         65.635
_diffrn_reflns_theta_min         3.112
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0750 before and 0.0481 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    1.255
_exptl_crystal_description       plate
_exptl_crystal_F_000             4091
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         8803
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.1079
_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^)+(0.1423P)^2^+38.4170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2933
_refine_ls_wR_factor_ref         0.3034
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7293
_reflns_number_total             8803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13790_si_001.cif
_cod_data_source_block           Monomer
_cod_original_cell_volume        10481.8(8)
_cod_database_code               4134206
_shelx_shelxl_version_number     2014/7
_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, All O(H,H) groups
2. Restrained distances
 B2-F6
 1.38 with sigma of 0.02
 F9-F10
 2.26 with sigma of 0.04
 F11-F13
 2.26 with sigma of 0.04
 F11-F14
 2.24 with sigma of 0.04
 F7-F5
 2.26 with sigma of 0.04
 F8-F5
 2.26 with sigma of 0.04
 F7-F8
 2.26 with sigma of 0.04
 B4-F17 \\sim B4-F18
 with sigma of 0.02
3. Others
 Sof(F13)=Sof(F11)=Sof(F14)=1-FVAR(1)
 Sof(F10)=Sof(F15)=Sof(F12)=FVAR(1)
 Fixed Sof: F17(0.5) F18(0.5) F19(0.5) F5(0.5) F8(0.5) F6(0.5) F7(0.5)
 O1(0.33333) H1A(0.33333) H1B(0.33333)
4.a Free rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C11(H11A,H11B)
4.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
  C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
 C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'