Versatile assembly of p-carboxylatocalix[4]arene-O-alkyl ethers.
Kennedy, Stuart; Teat, Simon J.; Dalgarno, Scott J.; Dalton transactions (Cambridge, England : 2003) 39 (2010) 384–387; doi:10.1039/b914133b

data_7024274
_publ_section_title
;
 Versatile assembly of p-carboxylatocalix[4]arene-O-alkyl ethers.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              384
_journal_page_last               387
_journal_paper_doi               10.1039/b914133b
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         '2(C44 H48 O12), 9(C5 H5 N)'
_chemical_formula_sum            'C133 H141 N9 O24'
_chemical_formula_weight         2249.55
_chemical_name_common            8Py
_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                64.188(3)
_cell_angle_beta                 89.399(3)
_cell_angle_gamma                88.268(3)
_cell_formula_units_Z            2
_cell_length_a                   12.2237(6)
_cell_length_b                   22.4428(11)
_cell_length_c                   24.2799(12)
_cell_measurement_temperature    100(2)
_cell_volume                     5993.5(5)
_computing_cell_refinement       'Bruker SAINTv7.34a'
_computing_data_collection       'Bruker Apex 2'
_computing_data_reduction        'Bruker SAINTv7.34a'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0996
_diffrn_reflns_av_sigmaI/netI    0.1212
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30229
_diffrn_reflns_theta_full        19.84
_diffrn_reflns_theta_max         19.84
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.6010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2004 Bruker AXS, Manison, WI'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1531
_refine_ls_number_reflns         10894
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0606P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1378
_reflns_number_gt                5866
_reflns_number_total             10894
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b914133b.txt
_cod_data_source_block           8Py
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7024274