The Quest for Chain-Link Hydrogen-Bonded Capsules: Self-Assembly of C-Methyl Calix[4]resorcinarene with 5,5‘-Bipyrimidine
Barnes, Charles L.; Bosch, Eric; Crystal Growth & Design 5 (2005) 1049–; doi:10.1021/cg049639v

data_4504927
_publ_section_title
;
 The Quest for Chain-Link Hydrogen-Bonded Capsules:&#x2009; Self-Assembly
 of C-Methyl Calix[4]resorcinarene with 5,5&#x2018;-Bipyrimidine
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1049
_journal_paper_doi               10.1021/cg049639v
_journal_volume                  5
_journal_year                    2005
_chemical_formula_sum            'C63 H65 N9 O8'
_chemical_formula_weight         1076.24
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.9260(10)
_cell_angle_beta                 117.3390(10)
_cell_angle_gamma                115.9260(10)
_cell_formula_units_Z            2
_cell_length_a                   15.5432(11)
_cell_length_b                   15.8676(11)
_cell_length_c                   15.9170(11)
_cell_measurement_reflns_used    3614
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.1
_cell_measurement_theta_min      2.5
_cell_volume                     2927.4(4)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'omega 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  0.0415
_diffrn_reflns_av_sigmaI/netI    0.1065
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21044
_diffrn_reflns_theta_full        27.16
_diffrn_reflns_theta_max         27.16
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     762
_refine_ls_number_reflns         12618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1632
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0867P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1976
_reflns_number_gt                5654
_reflns_number_total             12618
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg049639vsi20050216_030033.cif
_cod_data_source_block           CYMPYR02
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4504927