Chloride Selective Macrocyclic Bisurea Derivatives with 2,2'-Binaphthalene Moieties as Spacers.
Satake, Akira; Ishizawa, Yuki; Katagiri, Hiroshi; Kondo, Shin-Ichi; The Journal of organic chemistry 81 (2016) 9848–9857; doi:10.1021/acs.joc.6b01959

data_4037310
_publ_section_title
;
 Chloride Selective Macrocyclic Bisurea Derivatives with
 2,2'-Binaphthalene Moieties as Spacers.
;
_journal_issue                   20
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              9848
_journal_page_last               9857
_journal_paper_doi               10.1021/acs.joc.6b01959
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C58 H60 N4 O2, 1/3(C2 H6 O S)'
_chemical_formula_sum            'C58.66667 H62 N4 O2.33333 S0.33333'
_chemical_formula_weight         871.14
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.536(4)
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   31.448(8)
_cell_length_b                   17.914(4)
_cell_length_c                   72.329(18)
_cell_measurement_reflns_used    18849
_cell_measurement_temperature    113
_cell_measurement_theta_max      30.2
_cell_measurement_theta_min      10.2
_cell_volume                     40670(17)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.0761
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_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       86
_diffrn_reflns_limit_l_min       -86
_diffrn_reflns_number            110054
_diffrn_reflns_point_group_measured_fraction_full 0.911
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.032
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(REQAB; Jacobson, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    0.854
_exptl_crystal_description       Prism
_exptl_crystal_F_000             11184
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         32635
_refine_ls_number_restraints     607
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0847
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1633P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2609
_refine_ls_wR_factor_ref         0.2837
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20137
_reflns_number_total             32635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b01959_si_002.cif
_cod_data_source_block           1498499
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 

2025-10-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C176 H186 N12 O7 S'
_cod_original_formula_weight         2613.42
_cod_original_formula_moiety         '3(C58 H60 N4 O2), C2 H6 O S'
_cod_original_formula_units_Z            8
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4037310
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              2549
_shelx_hkl_checksum              47146
_shelx_fab_checksum              82225