A Synthetic Route for Crystals of Woven Structures, Uniform Nanocrystals, and Thin Films of Imine Covalent Organic Frameworks.
Zhao, Yingbo; Guo, Lei; Gándara, Felipe; Ma, Yanhang; Liu, Zheng; Zhu, Chenhui; Lyu, Hao; Trickett, Christopher A.; Kapustin, Eugene A.; Terasaki, Osamu; Yaghi, Omar M.; Journal of the American Chemical Society 139 (2017) 13166–13172; doi:10.1021/jacs.7b07457

data_4131604
_publ_section_title
;
 A Synthetic Route for Crystals of Woven Structures, Uniform Nanocrystals,
 and Thin Films of Imine Covalent Organic Frameworks.
;
_journal_issue                   37
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13166
_journal_page_last               13172
_journal_paper_doi               10.1021/jacs.7b07457
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C38 H34 Co N10, 2(B F4), 2(C2 H3 N)'
_chemical_formula_sum            'C42 H40 B2 Co F8 N12'
_chemical_formula_weight         945.41
_chemical_name_common
'Bis-2,6-pyridinedicarboxaldhydebis(p-aminophenylimine) cobalt tetrafluoroborate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                113.528(4)
_cell_angle_beta                 90.375(4)
_cell_angle_gamma                112.600(4)
_cell_formula_units_Z            2
_cell_length_a                   12.1126(16)
_cell_length_b                   14.208(2)
_cell_length_c                   15.083(2)
_cell_measurement_reflns_used    4108
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.683
_cell_measurement_theta_min      2.354
_cell_volume                     2157.6(5)
_computing_cell_refinement       'SAINT V8.37A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.37A Bruker-AXS, Madison WI'
_computing_molecular_graphics
;
Bruker SHELXTL Bruker-AXS, Madison WI
and local programs
;
_computing_publication_material  'Bruker SHELXTL Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 Bruker-AXS, Madison WI'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.1378
_diffrn_reflns_av_unetI/netI     0.0885
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3913
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        21.650
_diffrn_reflns_theta_max         21.709
_diffrn_reflns_theta_min         2.101
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.6023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.2191 before and 0.0850 after correction. The Ratio of minimum to maximum transmission is 0.8088. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       Block
_exptl_crystal_F_000             970
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         3913
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.0810
_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^)+(0.0605P)^2^+27.3741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1841
_refine_ls_wR_factor_ref         0.2050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2898
_reflns_number_total             3913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07457_si_003.cif
_cod_data_source_block           yzsu
_cod_original_cell_volume        2157.7(5)
_cod_database_code               4131604
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.982
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N2 \\sim C12 \\sim C11 \\sim C13: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C36) = Uanis(N7)
3. Rigid body (RIGU) restrains
 N7, C36, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C12, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, N5
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Co1, N6, C32, C31, N5
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Rotating group:
 N7(H7A,H7B), N10(H10A,H10B), N8(H8A,H8B), N9(H9A,H9B)
4.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C2(H2), C26(H26), C25(H25), C19(H19), C15(H15), C7(H7), C6(H6),
 C38(H38), C3(H3), C11(H11), C18(H18), C28(H28), C32(H32), C37(H37), C5(H5),
 C24(H24), C22(H22), C34(H34), C30(H30), C21(H21), C13(H13), C16(H16), C9(H9),
 C10(H10), C29(H29)
4.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              71491
_shelx_hkl_checksum              30719
_olex2_submission_special_instructions 'No special instructions were received'