Pyridine Directed Assembly of Tetra-O-Alkylp-Carboxylatocalix[4]arenes
Kennedy, Stuart; Beavers, Christine M.; Teat, Simon J.; Dalgarno, Scott J.; Crystal Growth & Design 12 (2012) 679–; doi:10.1021/cg2008864

data_4502760
_publ_section_title
;
 Pyridine Directed Assembly of Tetra-O-Alkylp-Carboxylatocalix[4]arenes
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              679
_journal_paper_doi               10.1021/cg2008864
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C62 H69 N3 O12'
_chemical_formula_weight         1048.20
_chemical_name_common            FINISHRK642Pic
_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                76.6590(10)
_cell_angle_beta                 69.1400(10)
_cell_angle_gamma                86.7000(10)
_cell_formula_units_Z            2
_cell_length_a                   13.1917(11)
_cell_length_b                   15.0871(12)
_cell_length_c                   15.4152(13)
_cell_measurement_temperature    100(2)
_cell_volume                     2788.5(4)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'Apex II'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD Diffractometer'
_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     0.77490
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_sigmaI/netI    0.0816
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33369
_diffrn_reflns_theta_full        30.23
_diffrn_reflns_theta_max         30.23
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.9957
_exptl_absorpt_correction_T_min  0.9829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         12730
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0426P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1624
_refine_ls_wR_factor_ref         0.1804
_reflns_number_gt                7816
_reflns_number_total             12730
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2008864_si_002.cif
_cod_data_source_block           72Pic
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4502760