Pyridine Directed Assembly of Di-O-Alkyl-tris-p-Carboxylatocalix[4]arenes
Kennedy, Stuart; Dodgson, India E.; Beavers, Christine M.; Teat, Simon J.; Dalgarno, Scott J.; Crystal Growth & Design 12 (2012) 688–; doi:10.1021/cg200887d

data_4502773
_publ_section_title
;
 Pyridine Directed Assembly of Di-O-Alkyl-tris-p-Carboxylatocalix[4]arenes
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              688
_journal_paper_doi               10.1021/cg200887d
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C119 H127 N7 O20'
_chemical_formula_weight         1975.28
_chemical_name_common            FINISHSRKRK752EtPy
_chemical_name_systematic
;
 ?
;
_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                65.185(2)
_cell_angle_beta                 76.938(2)
_cell_angle_gamma                68.755(2)
_cell_formula_units_Z            2
_cell_length_a                   16.2735(19)
_cell_length_b                   19.252(2)
_cell_length_c                   19.904(2)
_cell_measurement_temperature    100(2)
_cell_volume                     5255.3(10)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex II CCD Diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_sigmaI/netI    0.0791
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33137
_diffrn_reflns_theta_full        22.34
_diffrn_reflns_theta_max         22.34
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.9983
_exptl_absorpt_correction_T_min  0.9915
_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             2100
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.146
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1327
_refine_ls_number_reflns         10349
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1921
_refine_ls_wR_factor_ref         0.2314
_reflns_number_gt                6200
_reflns_number_total             10349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200887d_si_002.cif
_cod_data_source_block           42EtPy
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4502773