Hexameric assembly of 5,17-di-substituted calix[4]arene in the solid state
Yamasaki, Yutaro; Sekiya, Ryo; Haino, Takeharu; CrystEngComm  (2017) –; doi:10.1039/C7CE01515A

data_7229529
_publ_section_title
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 Hexameric assembly of 5,17-di-substituted calix[4]arene in the solid
 state
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01515A
_journal_year                    2017
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C56 H62 N2 O8 (C3H8O)'
_chemical_formula_sum            'C59 H70 N2 O9'
_chemical_formula_weight         951.17
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-10-25T17:25:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-10-26 deposited with the CCDC.
2017-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.5600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.587(2)
_cell_length_b                   9.5507(8)
_cell_length_c                   19.5075(15)
_cell_measurement_reflns_used    6280
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.54
_cell_measurement_theta_min      2.28
_cell_volume                     5223.6(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2017 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Bluker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15902
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.124
_diffrn_reflns_theta_min         2.157
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2044
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 3135 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         10913
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+6.1356P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.588
_reflns_Friedel_fraction_full    0.755
_reflns_Friedel_fraction_max     0.61
_reflns_number_gt                9273
_reflns_number_total             10913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01515a2.cif
_cod_data_source_block           2PrOH
_cod_depositor_comments
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The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7229529
_shelx_res_checksum              50516