The crystal structure of 25,27-(2,2′-[(2-thioxo-1,3-dithiole-4,5-diyl)disulfanediyl]diethanolate)-26,28-dihydroxycalix[4]arene — dichloromethane (1/1), C36H32Cl2O4S5
Liu, Lian-Wei; Zhong, Ji-Yan; Zhao, Bang-Tun; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 67–68; doi:10.1515/ncrs-2017-0154

data_8106045
_publ_section_title
;
 The crystal structure of
 25,27-(2,2&#x2032;-[(2-thioxo-1,3-dithiole-4,5-diyl)disulfanediyl]diethanolate)-26,28-dihydroxycalix[4]arene
 --- dichloromethane (1/1), C36H32Cl2O4S5
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              67
_journal_page_last               68
_journal_paper_doi               10.1515/ncrs-2017-0154
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C35 H30 O4 S5, C H2 Cl2'
_chemical_formula_sum            'C36 H32 Cl2 O4 S5'
_chemical_formula_weight         759.82
_chemical_name_systematic
;
25,27-(2,2'-[(2-thioxo-1,3-dithiole-4,5-diyl)disulfanediyl]diethanolate)
-26,28-dihydroxycalix[4]arene dichloromethane solvate
;
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.4426(11)
_cell_length_b                   17.4623(13)
_cell_length_c                   25.9153(19)
_cell_measurement_reflns_used    8336
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      24.24
_cell_measurement_theta_min      2.36
_cell_volume                     6988.4(9)
_computing_cell_refinement       'Bruker SMART [1-2]'
_computing_data_collection       'Bruker SMART [1-2]'
_computing_data_reduction        'Bruker SAINT [1-2]'
_computing_molecular_graphics    'Bruker SHELXTL [1-2]'
_computing_publication_material  'Bruker SHELXTL [1-2]'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997) [3]'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990) [3]'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  '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  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42129
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.9335
_exptl_absorpt_correction_T_min  0.8240
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         8015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0961P)^2^+5.1348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1958
_reflns_number_gt                4993
_reflns_number_total             8015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2017-0154_suppl.cif
_cod_data_source_block           a
_cod_original_sg_symbol_H-M      Pccn
_cod_database_code               8106045