Urea-Linked Covalent Organic Frameworks.
Zhao, Chenfei; Diercks, Christian S.; Zhu, Chenhui; Hanikel, Nikita; Pei, Xiaokun; Yaghi, Omar M.; Journal of the American Chemical Society 140 (2018) 16438–16441; doi:10.1021/jacs.8b10612

data_4133516
_publ_section_title
;
 Urea-Linked Covalent Organic Frameworks.
;
_journal_issue                   48
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16438
_journal_page_last               16441
_journal_paper_doi               10.1021/jacs.8b10612
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C30 H24 N6 O6, 3(C5 H9 N O)'
_chemical_formula_sum            'C45 H51 N9 O9'
_chemical_formula_weight         861.95
_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
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-09-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 116.386(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.4628(15)
_cell_length_b                   19.1378(10)
_cell_length_c                   14.8992(8)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.291
_cell_measurement_theta_min      2.214
_cell_volume                     8292.0(7)
_computing_cell_refinement       'SAINT V8.38A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker-AXS, Madison WI'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 2014/7 Bruker-AXS, Madison WI'
_computing_structure_solution    'SHELXT 2014/5 Bruker-AXS, Madison WI'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker PHOTON-100'
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'CMOS detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            70085
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        23.309
_diffrn_reflns_theta_max         23.309
_diffrn_reflns_theta_min         2.242
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1195 before and 0.0659 after correction. The Ratio of minimum to maximum transmission is 0.8788. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light red'
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.707
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         5989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0842
_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^)+(0.1630P)^2^+38.2960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2357
_refine_ls_wR_factor_ref         0.2604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4705
_reflns_number_total             5989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10612_si_002.cif
_cod_data_source_block           model_compound
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4133516
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.971
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C42(H42A,H42B), C37(H37A,H37B), C39(H39A,H39B), C34(H34A,
 H34B), C43(H43A,H43B), C32(H32A,H32B), C38(H38A,H38B), C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), N6(H6), N3(H3), N1(H1), N5(H5), C7(H7), C15(H15), C23(H23),
 C30(H30), C10(H10), C14(H14), C11(H11), C13(H13), C26(H26), C20(H20), C12(H12),
  C27(H27), C18(H18), C29(H29), C19(H19), C28(H28), C22(H22), C21(H21)
2.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C35(H35A,H35B,H35C), C45(H45A,H45B,H45C)
;
_olex2_submission_special_instructions 'No special instructions were received'