From 2 + 2 to 8 + 8 Condensation Products of Diamine and Dialdehyde: Giant Container-Shaped Macrocycles for Multiple Anion Binding.
Gregoliński, Janusz; Ślepokura, Katarzyna; Paćkowski, Tomasz; Panek, Jarosław; Stefanowicz, Piotr; Lisowski, Jerzy; The Journal of organic chemistry 81 (2016) 5285–5294; doi:10.1021/acs.joc.6b00531

data_4036793
_publ_section_title
;
 From 2 + 2 to 8 + 8 Condensation Products of Diamine and Dialdehyde:
 Giant Container-Shaped Macrocycles for Multiple Anion Binding.
;
_journal_issue                   13
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5285
_journal_page_last               5294
_journal_paper_doi               10.1021/acs.joc.6b00531
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C48 H76 N12, 8(Cl), 4(H2 O)'
_chemical_formula_sum            'C48 H84 Cl8 N12 O4'
_chemical_formula_weight         1176.87
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_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                78.23(3)
_cell_angle_beta                 83.88(3)
_cell_angle_gamma                66.76(3)
_cell_formula_units_Z            2
_cell_length_a                   12.688(3)
_cell_length_b                   12.980(4)
_cell_length_c                   20.266(6)
_cell_measurement_reflns_used    9210
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      2.89
_cell_volume                     3001.1(16)
_computing_cell_refinement
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
;
Kuma KM4-CCD kappa-geometry diffractometer 
with a Sapphire2 CCD camera 
;
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.993
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_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22432
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         2.897
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.093
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         11091
_refine_ls_number_restraints     734
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1293
_refine_ls_R_factor_gt           0.0919
_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^)+(0.1862P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2644
_refine_ls_wR_factor_ref         0.2868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7067
_reflns_number_total             11091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b00531_si_002.cif
_cod_data_source_block           3c'_l44
_cod_database_code               4036793
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.883
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              23191
_shelx_hkl_checksum              36594