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_7024275
_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
'C48 H56 O12, 0.5(C12 H12), 4(C5 H5 N), 0.5(C6 H6)'
_chemical_formula_sum            'C77 H85 N4 O12'
_chemical_formula_weight         1258.49
_chemical_name_common            9Py
_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                92.18(3)
_cell_angle_beta                 100.82(3)
_cell_angle_gamma                99.60(3)
_cell_formula_units_Z            2
_cell_length_a                   12.236(2)
_cell_length_b                   13.141(3)
_cell_length_c                   22.319(5)
_cell_measurement_temperature    100(2)
_cell_volume                     3466.7(13)
_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 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker Nonius X8 Apex 2'
_diffrn_measurement_method       'omega and phi 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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34541
_diffrn_reflns_theta_full        21.46
_diffrn_reflns_theta_max         21.46
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.6814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1342
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         7628
_refine_ls_number_restraints     360
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0809P)^2^+5.4870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.1718
_reflns_number_gt                5602
_reflns_number_total             7628
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b914133b.txt
_cod_data_source_block           9Py
_cod_original_cell_volume        3466.7(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7024275