A Two-Dimensional Polymer Synthesized through Topochemical [2 + 2]-Cycloaddition on the Multigram Scale.
Lange, Ralph Z.; Hofer, Gregor; Weber, Thomas; Schlüter, A Dieter; Journal of the American Chemical Society 139 (2017) 2053–2059; doi:10.1021/jacs.6b11857

data_4125590
_publ_section_title
;
 A Two-Dimensional Polymer Synthesized through Topochemical [2 +
 2]-Cycloaddition on the Multigram Scale.
;
_journal_issue                   5
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2053
_journal_page_last               2059
_journal_paper_doi               10.1021/jacs.6b11857
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C23 H27 O, B F4, H2 O'
_chemical_formula_sum            'C23 H29 B F4 O2'
_chemical_formula_weight         424.27
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-07-22
_audit_creation_method
;
Olex2 1.2
(compiled Feb 16 2016 13:09:46 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   27.2965(7)
_cell_length_b                   27.2965(7)
_cell_length_c                   16.2071(6)
_cell_measurement_reflns_used    27483
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.02
_cell_measurement_theta_min      3
_cell_volume                     10458.0(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_device_type  'BM01a at ESRF'
_diffrn_measurement_method       Transmission
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6935
_diffrn_reflns_av_R_equivalents  0.1185
_diffrn_reflns_av_unetI/netI     0.0751
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27483
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        24.589
_diffrn_reflns_theta_max         32.018
_diffrn_reflns_theta_min         2.081
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       Rhombohedra
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          500
_exptl_crystal_size_mid          450
_exptl_crystal_size_min          400
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         7469
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      2.159
_refine_ls_R_factor_all          0.1938
_refine_ls_R_factor_gt           0.1724
_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          0.5211
_refine_ls_wR_factor_ref         0.5422
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5236
_reflns_number_total             7469
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b11857_si_001.cif
_cod_data_source_block           mono_syn
_cod_depositor_comments          'Adding full bibliography for 4125590.cif.'
_cod_original_cell_volume        10458.0(7)
_cod_database_code               4125590
_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
 C23A-C22A
 2.5 with sigma of 0.02
 C23A-C24A
 2.5 with sigma of 0.02
 C24A-C22A
 2.5 with sigma of 0.02
 F3A-F2A
 2.35 with sigma of 0.02
 F2A-F4A
 2.35 with sigma of 0.02
 F4A-F3A
 2.35 with sigma of 0.02
 C21A-C23A \\sim C21A-C24A \\sim C21A-C22A \\sim C0AA-C1AA \\sim C0AA-C2AA
\\sim C0AA-C3AA
 with sigma of 0.02
 O1-C14 \\sim O1-C15
 with sigma of 0.02
 C12A-C14 \\sim C12A-C11A \\sim C1BA-C0AB \\sim C13A-C11A
 with sigma of 0.02
 C4AA-C6AA \\sim C4AA-C7AA \\sim C21A-C23A \\sim C4AA-C5AA \\sim C21A-C22A
\\sim C21A-C24A
 with sigma of 0.02
 C0AA-C2AA \\sim C17A-C20A \\sim C0AA-C3AA \\sim C17A-C19A \\sim C17A-C18A
 with sigma of 0.02
 C17A-C15 \\sim C4AA-C14
 with sigma of 0.02
 F3A-B1 \\sim F4A-B1 \\sim F2A-B1 \\sim F1A-B1
 with sigma of 0.02
 C13A-C11A \\sim C13A-C15 \\sim C1BA-C0AB \\sim C12A-C11A \\sim C1BA-C14 \\sim
C12A-C14
 with sigma of 0.02
 F3B-B1B \\sim F3A-B1 \\sim F4B-B1B \\sim F1B-B1B \\sim F2A-B1 \\sim F1A-B1
\\sim F4A-B1 \\sim F2B-B1B
 with sigma of 0.02
 O1-C15 \\sim O1-C14
 with sigma of 0.02
 C13A-C15 \\sim C12A-C14 \\sim C1BA-C0AB \\sim C12A-C11A \\sim C13A-C11A \\sim
C6-C4 \\sim C6-C8 \\sim C8-
 C7 \\sim C5-C7 \\sim C5-C3 \\sim C3-C4 \\sim C1-C2
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uiso(C1BA) = Uiso(C0AB) = Uiso(C21A) = Uiso(C17A)
Uiso(C4AA) = Uiso(C12A) = Uiso(C11A) = Uiso(C13A) = Uiso(C0AA)
Uiso(C24A) = Uiso(C23A) = Uiso(C22A)
Uiso(C6AA) = Uiso(C5AA) = Uiso(C7AA)
Uiso(C1AA) = Uiso(C3AA) = Uiso(C2AA)
Uiso(C19A) = Uiso(C20A) = Uiso(C18A)
4. Rigid body (RIGU) restrains
 F1A, B1, F4A, F3A, F2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H13B)=Sof(C7A)=Sof(H7A)=Sof(C4AB)=Sof(H4AB)=Sof(C0AB)=Sof(C1BA)=Sof(H1BA)=
 Sof(C21A)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C24A)=Sof(H24A)=
 Sof(H24B)=Sof(H24C)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C17A)=
 Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19A)=Sof(H19A)=Sof(H19B)=
 Sof(H19C)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(H20C)=1-FVAR(1)
 Sof(H13A)=Sof(C12A)=Sof(H12A)=Sof(C11A)=Sof(C10A)=Sof(H10A)=Sof(C0AA)=
 Sof(C4AA)=Sof(C9A)=Sof(H9A)=Sof(C5AA)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C3AA)=
 Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C6AA)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=
 Sof(C7AA)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=
 Sof(H2AC)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=FVAR(1)
 Sof(F4B)=Sof(F1B)=Sof(B1B)=Sof(F2B)=Sof(F3B)=1-FVAR(2)
 Sof(F1A)=Sof(B1)=Sof(F4A)=Sof(F3A)=Sof(F2A)=FVAR(2)
6.a Free rotating group:
 O2(H2A,H2B)
6.b Ternary CH refined with riding coordinates:
 C7A(H7A), C4AB(H4AB)
6.c Aromatic/amide H refined with riding coordinates:
 C13A(H13A), C13A(H13B), C1(H1), C5(H5), C12A(H12A), C7(H7), C4(H4),
 C10A(H10A), C6(H6), C9A(H9A), C1BA(H1BA)
6.d Idealised Me refined as rotating group:
 C5AA(H5AA,H5AB,H5AC), C3AA(H3AA,H3AB,H3AC), C6AA(H6AA,H6AB,H6AC), C7AA(H7AA,
 H7AB,H7AC), C2AA(H2AA,H2AB,H2AC), C1AA(H1AA,H1AB,H1AC), C22A(H22A,H22B,H22C),
 C24A(H24A,H24B,H24C), C23A(H23A,H23B,H23C), C18A(H18A,H18B,H18C), C19A(H19A,
 H19B,H19C), C20A(H20A,H20B,H20C)
;
_shelx_res_checksum              80568
_shelx_hkl_checksum              98305
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'