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_4037312
_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, C16 H36 N, 0.5(C2 H6 O S), Cl'
_chemical_formula_sum            'C75 H102 Cl N5 O2.5 S0.5'
_chemical_formula_weight         1165.10
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/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                 95.6897(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.4480(6)
_cell_length_b                   16.3547(3)
_cell_length_c                   24.2238(4)
_cell_measurement_reflns_used    75980
_cell_measurement_temperature    203
_cell_measurement_theta_max      68.24
_cell_measurement_theta_min      3.00
_cell_volume                     13580.1(4)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2003)'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996) and PLATON (Spek, 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita, 2001, Kabuto et al., 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      203
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            118268
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    1.011
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5056
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.002
_refine_diff_density_min         -0.001
_refine_diff_density_rms         0.000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     861
_refine_ls_number_reflns         12075
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1103P)^2^+0.0001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1830
_refine_ls_wR_factor_ref         0.2357
_reflns_number_gt                7704
_reflns_number_total             12075
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo6b01959_si_002.cif
_cod_data_source_block           1498502
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' 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 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C75 H102 Cl N5 O2.50 S0.50'
_cod_database_code               4037312