Temperature-dependent self-assembly of a purely organic cage in water.
Zheng, Xujun; Zhang, Yang; Wu, Guangcheng; Liu, Ji-Ren; Cao, Ning; Wang, Lei; Wang, Yan; Li, Xiaopeng; Hong, Xin; Yang, Chuluo; Li, Hao; Chemical communications (Cambridge, England) 54 (2018) 3138–3141; doi:10.1039/c8cc01085d

data_7121345
_publ_section_title
;
 Temperature-dependent self-assembly of a purely organic cage in water.
;
_journal_issue                   25
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3138
_journal_page_last               3141
_journal_paper_doi               10.1039/c8cc01085d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         '2(F6 P), C15 H18 N6 O'
_chemical_formula_sum            'C15 H18 F12 N6 O P2'
_chemical_formula_weight         588.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-11-08
_audit_creation_method
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Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5381)
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_audit_update_record
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2018-02-28 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.506(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.1886(6)
_cell_length_b                   14.4194(15)
_cell_length_c                   25.629(3)
_cell_measurement_reflns_used    1870
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3868
_cell_measurement_theta_min      3.1790
_cell_volume                     2282.7(4)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -37.00   59.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4683   38.0000  150.0000 96

  2 omega  -34.00   46.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4683   38.0000  -90.0000 80
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0728957000
_diffrn_orient_matrix_UB_12      0.0236853000
_diffrn_orient_matrix_UB_13      -0.0156703000
_diffrn_orient_matrix_UB_21      -0.0191384000
_diffrn_orient_matrix_UB_22      -0.0333971000
_diffrn_orient_matrix_UB_23      -0.0200647000
_diffrn_orient_matrix_UB_31      -0.0866412000
_diffrn_orient_matrix_UB_32      0.0272709000
_diffrn_orient_matrix_UB_33      -0.0109758000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            9094
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.185
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       needle
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.0876
_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^)+(0.1618P)^2^+1.6687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2505
_refine_ls_wR_factor_ref         0.2955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2497
_reflns_number_total             4177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01085d2.cif
_cod_data_source_block           171107_zxj_bond
_cod_depositor_comments          'Adding full bibliography for 7121345.cif.'
_cod_database_code               7121345
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H N O p f'
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.913
_reflns_odcompleteness_completeness 99.55
_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) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), C1(H1), C2(H2), C3(H3A), C4(H4A), C6(H6), C8(H8), C10(H10),
 C11(H11), C12(H12), C13(H13)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              78309
_olex2_submission_special_instructions 'No special instructions were received'