Thermodynamics of pillararene·guest complexation: blinded dataset for the SAMPL9 challenge
Deng, Chun-Lin; Cheng, Ming; Zavalij, Peter Y.; Isaacs, Lyle; New Journal of Chemistry 46 (2022) 995–1002; doi:10.1039/D1NJ05209H

data_7061127
_publ_section_title
;
 Thermodynamics of pillararene&#x00B7;guest complexation: blinded dataset
 for the SAMPL9 challenge
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              995
_journal_page_last               1002
_journal_paper_doi               10.1039/D1NJ05209H
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C14 H30 N2, 2(I)'
_chemical_formula_sum            'C14 H30 I2 N2'
_chemical_formula_weight         480.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-08-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-08 deposited with the CCDC.	2021-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.2182(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.5208(2)
_cell_length_b                   14.5116(5)
_cell_length_c                   10.1283(3)
_cell_measurement_reflns_used    10015
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      2.5
_cell_volume                     929.05(5)
_computing_cell_refinement       'Apex2, Saint (Bruker, 2012)'
_computing_data_collection       'Apex2 (Bruker, 2012)'
_computing_data_reduction        'Apex2, Saint'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015c)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0559613
_diffrn_orient_matrix_UB_12      0.0008476
_diffrn_orient_matrix_UB_13      0.0834930
_diffrn_orient_matrix_UB_21      0.0225305
_diffrn_orient_matrix_UB_22      0.0681498
_diffrn_orient_matrix_UB_23      0.0076005
_diffrn_orient_matrix_UB_31      -0.1462490
_diffrn_orient_matrix_UB_32      0.0101746
_diffrn_orient_matrix_UB_33      -0.0578387
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16743
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.248
_diffrn_reflns_theta_min         2.505
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.375
_exptl_absorpt_correction_T_max  0.430
_exptl_absorpt_correction_T_min  0.303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Krause et al, 2015)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             468
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.214
_refine_diff_density_min         -1.103
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0284(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         3037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0181P)^2^+0.9586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0553
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2779
_reflns_number_total             3037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05209h2.cif
_cod_data_source_block           UM3483b
_cod_depositor_comments          'Adding full bibliography for 7061127.cif.'
_cod_database_code               7061127
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.486
_shelx_estimated_absorpt_t_min   0.283
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C4(H4)
1.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C3(H3A,H3B), C2(H2A,H2B)
1.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              4695
_olex2_submission_special_instructions 'No special instructions were received'