2-(4-Bromobenzyl)-5,11,17,23-tetra-<i>tert</i>-butyl-25,26,27,28-tetramethoxycalix[4]arene
Fischer, Conrad; Lin, Guisheng; Seichter, Wilhelm; Weber, Edwin; Acta Crystallographica Section E 65 (2009) o1704–; doi:10.1107/S1600536809023137

data_2222465
_publ_section_title
2-(4-Bromobenzyl)-5,11,17,23-tetra-<i>tert</i>-butyl-25,26,27,28-tetramethoxycalix[4]arene
_journal_coeditor_code           SU2121
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1704
_journal_paper_doi               10.1107/S1600536809023137
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C55 H69 Br O4'
_chemical_formula_moiety         'C55 H69 Br O4'
_chemical_formula_sum            'C55 H69 Br O4'
_chemical_formula_weight         874.01
_chemical_name_systematic
;
2-(4-Bromobenzyl)-5,11,17,23-tetra-<i>tert</i>-butyl-25,26,27,28-
tetramethoxycalix[4]arene
;
_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                86.473(2)
_cell_angle_beta                 80.442(3)
_cell_angle_gamma                67.171(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8146(5)
_cell_length_b                   13.8980(5)
_cell_length_c                   18.0582(8)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.82
_cell_measurement_theta_min      2.29
_cell_volume                     2466.82(19)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42636
_diffrn_reflns_theta_full        27.30
_diffrn_reflns_theta_max         27.30
_diffrn_reflns_theta_min         1.14
_diffrn_standards_decay_%        <1%
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.9175
_exptl_absorpt_correction_T_min  0.7319
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.381
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         11033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0738P)^2^+0.3917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1384
_reflns_number_gt                7504
_reflns_number_total             11033
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su2121.cif
_cod_data_source_block           I
_cod_original_cell_volume        2466.82(18)
_cod_database_code               2222465
_cod_database_fobs_code          2222465