25,27-(3,6,9-Trioxaundecane-1,11-dioxy)-26,28-[3-(4-tricyanoethylene)phenyl]-3-aza-pentane-1,5-dioxy)calix[4]arene dichloromethane monosolvate
Lee, Jae Myoung; Kim, Sung Baek; Sim, Wonbo; Lee, Jai Young; IUCrData 4 (2019) x190026–; doi:10.1107/S2414314619000269

data_1550462
_publ_section_title
;
 25,27-(3,6,9-Trioxaundecane-1,11-dioxy)-26,28-[3-(4-tricyanoethylene)phenyl]-3-aza-pentane-1,5-dioxy)calix[4]arene
 dichloromethane monosolvate
;
_journal_issue                   1
_journal_name_full               IUCrData
_journal_page_first              x190026
_journal_paper_doi               10.1107/S2414314619000269
_journal_volume                  4
_journal_year                    2019
_chemical_formula_sum            'C52 H50 Cl2 N4 O7'
_chemical_formula_weight         913.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 92.999(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.702(3)
_cell_length_b                   11.349(2)
_cell_length_c                   28.538(6)
_cell_measurement_reflns_used    5252
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.10
_cell_measurement_theta_min      2.29
_cell_volume                     4431.7(16)
_computing_cell_refinement
;
SMART and SAINT (Bruker, 2000)
;
_computing_data_collection
;
SMART (Bruker, 2000)
;
_computing_data_reduction
;
SAINT (Bruker, 2000)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
<i>SHELXL2018/1</i> (Sheldrick, 2015) and  publCIF (Westrip
2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/1</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_unetI/netI     0.1342
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            32433
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.333
_diffrn_reflns_theta_min         1.617
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.762
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         11032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.880
_refine_ls_R_factor_all          0.1665
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0639P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1754
_reflns_number_gt                4410
_reflns_number_total             11032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj4200sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        4431.4(15)
_cod_database_code               1550462
_cod_database_fobs_code          1550462
_shelx_estimated_absorpt_t_min   0.909
_shelx_estimated_absorpt_t_max   0.966
_shelx_hkl_checksum              61302
_shelx_res_checksum              75421