Exploring Applications of Covalent Organic Frameworks: Homogeneous Reticulation of Radicals for Dynamic Nuclear Polarization.
Cao, Wei; Wang, Wei David; Xu, Hai-Sen; Sergeyev, Ivan V.; Struppe, Jochem; Wang, Xiaoling; Mentink-Vigier, Frederic; Gan, Zhehong; Xiao, Ming-Xing; Wang, Lu-Yao; Chen, Guo-Peng; Ding, San-Yuan; Bai, Shi; Wang, Wei; Journal of the American Chemical Society 140 (2018) 6969–6977; doi:10.1021/jacs.8b02839

data_4132279
_publ_section_title
;
 Exploring Applications of Covalent Organic Frameworks: Homogeneous
 Reticulation of Radicals for Dynamic Nuclear Polarization.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6969
_journal_page_last               6977
_journal_paper_doi               10.1021/jacs.8b02839
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C24 H26 N3 O'
_chemical_formula_sum            'C24 H26 N3 O'
_chemical_formula_weight         372.48
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.4658(8)
_cell_length_b                   17.4658(8)
_cell_length_c                   15.8447(9)
_cell_measurement_reflns_used    941
_cell_measurement_temperature    295.35(10)
_cell_measurement_theta_max      19.3940
_cell_measurement_theta_min      4.0190
_cell_volume                     4833.5(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      295.35(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega    0.00   33.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2104   57.0000   60.0000 33

  2 omega   12.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2104   57.0000  -60.0000 77

  3 omega    0.00   25.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.6791  -99.0000   30.0000 25

  4 omega  -47.00   51.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2104  -77.0000  150.0000 98
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0386627000
_diffrn_orient_matrix_UB_12      0.0088233000
_diffrn_orient_matrix_UB_13      0.0095908000
_diffrn_orient_matrix_UB_21      0.0084551000
_diffrn_orient_matrix_UB_22      0.0396402000
_diffrn_orient_matrix_UB_23      -0.0027550000
_diffrn_orient_matrix_UB_31      -0.0090362000
_diffrn_orient_matrix_UB_32      -0.0005753000
_diffrn_orient_matrix_UB_33      -0.0436534000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0883
_diffrn_reflns_av_unetI/netI     0.1960
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11332
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.010
_diffrn_reflns_theta_min         3.689
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.024
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 460 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         4692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.2477
_refine_ls_R_factor_gt           0.1165
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1896P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2906
_refine_ls_wR_factor_ref         0.3798
_reflns_Friedel_coverage         0.903
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                1761
_reflns_number_total             4692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02839_si_002.cif
_cod_data_source_block           caowei0506
_cod_original_cell_volume        4833.5(5)
_cod_database_code               4132279
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Rotating group:
 N2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C16(H16), C17(H17), C19(H19),
 C20(H20)
2.c X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
2.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-05-08
_olex2_submission_special_instructions 'No special instructions were received'