Smart control of calixarene polymorphic states
Gabdulkhaev, Mukhammet Nafisovich; Ziganshin, Marat; Buzyurov, Aleksey V.; Schick, Christoph; Solovieva, Svetlana; Popova, Elena; Gubaidullin, Aidar Timergalievich; Gorbatchuk, Valery; CrystEngComm  (2020) –; doi:10.1039/D0CE01070G

data_7241241
_publ_section_title
;
 Smart control of calixarene polymorphic states
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01070G
_journal_year                    2020
_chemical_formula_moiety         'C72 H72 O8 S4, C3 H5 N'
_chemical_formula_sum            'C75 H77 N O8 S4'
_chemical_formula_weight         1248.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-07-21 deposited with the CCDC.	2020-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                67.348(7)
_cell_angle_beta                 79.935(7)
_cell_angle_gamma                78.053(9)
_cell_formula_units_Z            2
_cell_length_a                   14.764(3)
_cell_length_b                   14.966(3)
_cell_length_c                   16.677(4)
_cell_measurement_reflns_used    1578
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.42
_cell_measurement_theta_min      3.00
_cell_volume                     3308.5(12)
_computing_cell_refinement       'APEX2 v2008.6-1 (Bruker AXS)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0901
_diffrn_reflns_av_unetI/netI     0.2223
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24005
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.625
_diffrn_reflns_theta_min         2.370
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
G.M. Sheldrick (1998a). SADABS v.2.01, Bruker.
Siemens Area Detector Absorption Correction Program.
Bruker AXS. Madison. Wisconsin. USA
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       prism
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.574
_exptl_crystal_size_mid          0.271
_exptl_crystal_size_min          0.232
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0024(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         15508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.1783
_refine_ls_R_factor_gt           0.0837
_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^)+(0.0488P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7373
_reflns_number_total             15508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01070g2.cif
_cod_data_source_block           GVV_cx3_EtCN
_cod_original_cell_volume        3308.4(12)
_cod_database_code               7241241
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.955
_shelx_res_checksum              64131