Synthesis and Structure of Feet-to-Feet Connected Bisresorcinarenes.
Shimoyama, Daisuke; Ikeda, Toshiaki; Sekiya, Ryo; Haino, Takeharu; The Journal of organic chemistry 82 (2017) 13220–13230; doi:10.1021/acs.joc.7b02301

data_4033238
_publ_section_title
;
 Synthesis and Structure of Feet-to-Feet Connected Bisresorcinarenes.
;
_journal_issue                   24
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              13220
_journal_page_last               13230
_journal_paper_doi               10.1021/acs.joc.7b02301
_journal_volume                  82
_journal_year                    2017
_chemical_formula_moiety         'C104 H136 O16, 11(C3 H7 N O) '
_chemical_formula_sum            'C137 H213 N11 O27'
_chemical_formula_weight         2446.17
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-08-08T13:27:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.717(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.597(3)
_cell_length_b                   42.559(7)
_cell_length_c                   19.786(3)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      23.53
_cell_measurement_theta_min      2.15
_cell_volume                     13633(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.823
_diffrn_measured_fraction_theta_max 0.998
_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  0.0706
_diffrn_reflns_av_unetI/netI     0.059
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            114676
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.562
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       block
_exptl_crystal_F_000             5312
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.877
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1614
_refine_ls_number_reflns         20301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1163
_refine_ls_R_factor_gt           0.078
_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^)+(0.0811P)^2^+23.9133P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.19
_refine_ls_wR_factor_ref         0.2101
_reflns_Friedel_coverage         0
_reflns_number_gt                13380
_reflns_number_total             20301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b02301_si_002.cif
_cod_data_source_block           C14OHdmf_compound_1e_DMF
_cod_depositor_comments
;
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/ACS/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 

 Adding full bibliography for 4033235--4033239.cif.

2020-12-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C274 H426 N22 O54'
_cod_original_formula_weight         4892.34
_cod_original_formula_moiety         '2(C104 H136 O16), 22(C3 H7 N O) '
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4033238