Pillar[5]arenes with an introverted amino group: a hydrogen bonding tuning effect.
Chen, Lei; Li, Zhiming; Chen, Zhenxia; Hou, Jun-Li; Organic & biomolecular chemistry 11 (2013) 248–251; doi:10.1039/c2ob27044g

data_7152797
_publ_section_title
;
 Pillar[5]arenes with an introverted amino group: a hydrogen bonding
 tuning effect.
;
_journal_issue                   2
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              248
_journal_page_last               251
_journal_paper_doi               10.1039/c2ob27044g
_journal_volume                  11
_journal_year                    2013
_chemical_formula_sum            'C76 H94 N2 O29'
_chemical_formula_weight         1499.53
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.004(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.958(4)
_cell_length_b                   21.804(5)
_cell_length_c                   20.210(5)
_cell_measurement_reflns_used    3164
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.65
_cell_measurement_theta_min      2.22
_cell_volume                     8353(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1029
_diffrn_reflns_av_sigmaI/netI    0.1647
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            39475
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.9909
_exptl_absorpt_correction_T_min  0.9819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The disordered solvents of chloroformwithin the void were not crystallographically
well defined.

The SQUEEZE routine of the program PLATON was used
in order to eliminate the contribution of disordered solvents molecules,
thereby a final model based only on the ordered part of the crystal structure
was obtained.

The SQUEEZE routine suggested that
a total potential solvent area volume of 1278.4 Ang^3^,
and a void electron population of 271 per cell.
So the amount of the disordered solvent was 4 per cell suggested by electron count.
The overall formula should be (C76H94N2O29).(HCCL3), considering the contribution of solvent.

Refinement after the SQUEEZE routine gave significantly improved R values.
[R values before SQUEEZE]
R1 = 0.2667, wR2 = 0.6000, GooF = S = 1.994 for all data
;
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         14656
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.2456
_refine_ls_R_factor_gt           0.1409
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3690
_refine_ls_wR_factor_ref         0.4131
_reflns_number_gt                5493
_reflns_number_total             14656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ob27044g.txt
_cod_data_source_block           m20907b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7152797