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_7223957
_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 H50 N4 O20, 2(C H Cl3), C6'
_chemical_formula_sum            'C63 H52 Cl6 N4 O20'
_chemical_formula_weight         1397.79
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-29
_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                 122.480(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.236(3)
_cell_length_b                   15.7969(10)
_cell_length_c                   20.4001(19)
_cell_measurement_reflns_used    2791
_cell_measurement_temperature    170
_cell_measurement_theta_max      29.5320
_cell_measurement_theta_min      3.2491
_cell_volume                     6588.6(15)
_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      0.0317864000
_diffrn_orient_matrix_UB_12      0.0129120000
_diffrn_orient_matrix_UB_13      0.0300306000
_diffrn_orient_matrix_UB_21      -0.0116548000
_diffrn_orient_matrix_UB_22      0.0417624000
_diffrn_orient_matrix_UB_23      -0.0023522000
_diffrn_orient_matrix_UB_31      -0.0076135000
_diffrn_orient_matrix_UB_32      -0.0102306000
_diffrn_orient_matrix_UB_33      0.0281249000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13475
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.26
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94651
_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    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         6014
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0923P)^2^+5.5318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1856
_reflns_number_gt                4010
_reflns_number_total             6014
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra28117b2.cif
_cod_data_source_block           150728_ajg_d_008
_cod_original_cell_volume        6588.5(10)
_cod_database_code               7223957
_chemical_oxdiff_formula         'c10 h10 n2 o8'
_reflns_odcompleteness_completeness 99.53
_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, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Cl2 \\sim Cl1 \\sim C33 \\sim Cl3 \\sim H33 \\sim Cl3A \\sim Cl2A \\sim C33A
\\sim H33A \\sim Cl1A: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
3. Others
 Sof(Cl2A)=Sof(C33A)=Sof(H33A)=Sof(Cl3A)=Sof(Cl1A)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=Sof(C33)=Sof(H33)=FVAR(1)
 Fixed Sof: H28A(0.5) H28B(0.5) C32(0.5)
4.a Ternary CH refined with riding coordinates:
 C33(H33), C33A(H33A)
4.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C19(H19A,H19B), C28(H28A,H28B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C8(H8), C13(H13), C16(H16), C22(H22), C25(H25)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C)
4.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;