Synthesis and crystal structure of [2 + 2] calixsalens.
Srimurugan, Sankareswaran; Viswanathan, Balasubramanian; Varadarajan, Thirukallam Kanthadai; Varghese, Babu; Organic & biomolecular chemistry 4 (2006) 3044–3047; doi:10.1039/b604003a

data_7151227
_publ_section_title
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 Synthesis and crystal structure of [2 + 2] calixsalens.
;
_journal_issue                   16
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3044
_journal_page_last               3047
_journal_paper_doi               10.1039/b604003a
_journal_volume                  4
_journal_year                    2006
_chemical_absolute_configuration ad
_chemical_formula_moiety
'(C40 H40 N4 O8 S2), 1.33(C H2 Cl2), 0.66(C2 H6 O), (H2 O)'
_chemical_formula_sum            'C42.67 H48.67 Cl2.67 N4 O9.67 S2'
_chemical_formula_weight         930.84
_chemical_name_systematic
;
?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.42(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   27.55(2)
_cell_length_b                   10.928(8)
_cell_length_c                   23.154(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     6971(8)
_computing_cell_refinement       'cad4 system software'
_computing_data_collection       'cad4 system software'
_computing_data_reduction        'XCAD4 (WINGX)'
_computing_molecular_graphics    'ORTEP32 (WINGX)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'XCAD4 (WINGX)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'cad4 diffractometer'
_diffrn_measurement_method       'omega twotheta'
_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  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0873
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            7159
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '1 hour'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  0.9968
_exptl_absorpt_correction_T_min  0.8127
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was 3
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2924
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         6480
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.1477
_refine_ls_R_factor_gt           0.0872
_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^)+(0.1808P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2237
_refine_ls_wR_factor_ref         0.2484
_reflns_number_gt                3413
_reflns_number_total             6480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b604003a.txt
_cod_data_source_block           muru
_cod_original_sg_symbol_H-M      C2
_cod_database_code               7151227
_exptl_absorpt_factor_mur        0.000