Crystal structures of the HCl salts of pseudopeptidic macrocycles display "knobs into holes" hydrophobic interactions between aliphatic side chains
Alfonso, Ignacio; Bolte, Michael; Bru, Miriam; Burguete, M. Isabel; Luis, Santiago V.; CrystEngComm 11 (2009) 735–738; doi:10.1039/b821772f

data_7200764
_publ_section_title
;
 Crystal structures of the HCl salts of pseudopeptidic macrocycles display
 "knobs into holes" hydrophobic interactions between aliphatic side chains
;
_journal_coden_ASTM              CRECF4
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              735
_journal_page_last               738
_journal_paper_doi               10.1039/b821772f
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C44 H80 Cl4 N8 O6'
_chemical_formula_weight         958.96
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.299(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   26.413(5)
_cell_length_b                   7.1135(10)
_cell_length_c                   15.775(3)
_cell_measurement_reflns_used    4971
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.4
_cell_measurement_theta_min      3.9
_cell_volume                     2946.1(9)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997) '
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990) '
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_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  0.2331
_diffrn_reflns_av_sigmaI/netI    0.2101
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14292
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_T_max  0.9782
_exptl_absorpt_correction_T_min  0.9479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS (Spek, 2003; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.074
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.3(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.234
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5225
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.235
_refine_ls_R_factor_all          0.2316
_refine_ls_R_factor_gt           0.1420
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3132
_refine_ls_wR_factor_ref         0.3527
_reflns_number_gt                2281
_reflns_number_total             5225
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            B821772F.txt
_cod_data_source_block           miriam4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

 Replaced the incorrect bibliographical reference to the original
 publication with a proper one.

 Antanas Vaitkus,
 2019-09-18
;
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7200764