Halo-Derivatised Calix[4]tubes
Matthews, Susan E.; Felix, Vitor; Drew, Michael G. B.; Beer, Paul D.; Organic & Biomolecular Chemistry 1 (2003) 1232–; doi:10.1039/b211303a

data_7151384
_publ_section_title
;
 Halo-Derivatised Calix[4]tubes
;
_journal_issue                   7
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              1232
_journal_paper_doi               10.1039/b211303a
_journal_volume                  1
_journal_year                    2003
_chemical_formula_sum            'C109 H114 Br4 O7'
_chemical_formula_weight         1855.64
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 98.546(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.85(4)
_cell_length_b                   13.692(19)
_cell_length_c                   47.55(6)
_cell_measurement_temperature    293(2)
_cell_volume                     21150(5)
_computing_cell_refinement       XDS
_computing_data_collection       'XDS (Kabsch, 1991)'
_computing_data_reduction        XDS
_computing_molecular_graphics    PLATON(Spek,1994)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Marresearch Image Plate'
_diffrn_measurement_method
'95 frames at 2^o intervals, counting time 5 min.'
_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  0.0910
_diffrn_reflns_av_sigmaI/netI    0.3211
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            21071
_diffrn_reflns_theta_max         22.60
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    1.572
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.441
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7712
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.00025(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         12553
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.2825
_refine_ls_R_factor_gt           0.1262
_refine_ls_shift/su_max          0.102
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1553P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3100
_refine_ls_wR_factor_ref         0.3511
_reflns_number_gt                3433
_reflns_number_total             12553
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211303a.txt
_cod_data_source_block           12
_cod_original_cell_volume        21151(49)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7151384