Self-inclusion structure of 5,11,17,23-tetrakis(azidomethyl)-25,26,27,28-tetrahydroxycalix[4]arene, and 5,11,17,23-tetra-<i>tert</i>-butyl-25,27-bis(chloroacetoxy)-26,28-bis(2-pyridylmethoxy)calix[4]arene
Zhao, Mei; Zhang, Xin-Yan; Ma, Jian-Ping; Huang, Ru-Qi; Guo, Dian-Shun; Acta Crystallographica Section C 65 (2009) o186–o190; doi:10.1107/S0108270109010609

data_2017058
_publ_section_title
;Self-inclusion structure of
 5,11,17,23-tetrakis(azidomethyl)-25,26,27,28-tetrahydroxycalix[4]arene, and
 5,11,17,23-tetra-<i>tert</i>-butyl-25,27-bis(chloroacetoxy)-26,28-bis(2-pyridylmethoxy)calix[4]arene
;
_journal_coeditor_code           LN3123
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o186
_journal_page_last               o190
_journal_paper_doi               10.1107/S0108270109010609
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C32 H27.91 N11.73 O4.09'
_chemical_formula_moiety         '0.91(C32 H28 N12 O4), 0.09(C32 H27 N9 O5)'
_chemical_formula_sum            'C32 H27.91 N11.73 O4.09'
_chemical_formula_weight         642.20
_chemical_name_systematic
;
5,11,17,23-tetrakis(azidomethyl)-25,26,27,28-tetrahydroxycalix[4]arene
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.812(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.377(2)
_cell_length_b                   12.446(2)
_cell_length_c                   19.979(3)
_cell_measurement_reflns_used    3158
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.125
_cell_measurement_theta_min      2.362
_cell_volume                     2975.4(8)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Version 6.12; Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Version 6.12; Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega 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  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14693
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1339.1
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         5228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0819P)^2^+1.3905P] whereP=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1677
_reflns_number_gt                3717
_reflns_number_total             5228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ln3123.cif
_cod_data_source_block           I
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2975.3(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2017058
_cod_database_fobs_code          2017058