Pillar[5]arene derivatives containing two dinitrophenyl rings: Syntheses, conformations and the tubular self assembly in the solid state
Xue, Min; Xu, Xiaoyan; An, Jianggen; Wang, Jie; Yang, Yong; Liu, Yongsong; RSC Adv.  (2016) –; doi:10.1039/C5RA28117B

data_7223956
_publ_section_title
;
 Pillar[5]arene derivatives containing two dinitrophenyl rings: Syntheses,
 conformations and the tubular self assembly in the solid state
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA28117B
_journal_year                    2016
_chemical_formula_moiety         'C55 H48 F2 N4 O18, 2(C H2 Cl2)'
_chemical_formula_sum            'C57 H52 Cl4 F2 N4 O18'
_chemical_formula_weight         1260.83
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2015-12-25 deposited with the CCDC.
2016-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.511(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9412(5)
_cell_length_b                   15.9438(6)
_cell_length_c                   37.9153(15)
_cell_measurement_reflns_used    5256
_cell_measurement_temperature    170
_cell_measurement_theta_max      29.5631
_cell_measurement_theta_min      2.7739
_cell_volume                     6457.1(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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      170
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0200038000
_diffrn_orient_matrix_UB_12      -0.0362280000
_diffrn_orient_matrix_UB_13      0.0089547000
_diffrn_orient_matrix_UB_21      -0.0575405000
_diffrn_orient_matrix_UB_22      0.0193464000
_diffrn_orient_matrix_UB_23      0.0019250000
_diffrn_orient_matrix_UB_31      -0.0226855000
_diffrn_orient_matrix_UB_32      -0.0170770000
_diffrn_orient_matrix_UB_33      -0.0168363000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            29158
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76766
_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    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.26
_platon_squeeze_details
;
;
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         11789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0980P)^2^+3.8006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.2005
_reflns_number_gt                8961
_reflns_number_total             11789
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra28117b2.cif
_cod_data_source_block           150414_xxy_019_2
_cod_database_code               7223956
_chemical_oxdiff_formula         'c10 h10 n2 o8 f3'
_reflns_odcompleteness_completeness 99.59
_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 C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C16(H16A,H16B), C25(H25A,H25B), C34(H34A,H34B), C43(H43A,H43B),
 C56(H56A,H56B), C57(H57A,H57B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C10(H10), C13(H13), C19(H19), C22(H22), C28(H28), C31(H31),
 C37(H37), C40(H40), C45(H45), C48(H48), C51(H51), C54(H54)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C)
;