7,11,15,28-Tetrakis(bromomethyl)-1,21,23,25-tetrapentylresorcin[4]arene cavitand 0.415-hydrate
McKay, Michael G.; Friedrich, Holger B.; Maguire, Glenn E. M.; Acta Crystallographica Section E 63 (2007) o4345–o4345; doi:10.1107/S1600536807050106

data_2215973
_publ_section_title
;
 7,11,15,28-Tetrakis(bromomethyl)-1,21,23,25-tetrapentylresorcin[4]arene
 cavitand 0.415-hydrate
;
_journal_coeditor_code           HG2300
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4345
_journal_page_last               o4345
_journal_paper_doi               10.1107/S1600536807050106
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C56 H68 Br4 O8, 0.415H2 O'
_chemical_formula_moiety         'C56 H68 Br4 O8, 0.415(H2 O)'
_chemical_formula_sum            'C56 H68.83 Br4 O8.41'
_chemical_formula_weight         1197.75
_chemical_melting_point          553
_chemical_name_common
;
7,11,15,28-Tetrakis(bromomethyl)-1,21,23,25-
tetrapentyl-resorcin[4]arene cavitand
;
_chemical_name_systematic
;
7,11,15,28-tetrakis(bromomethyl)-1,21,23,25-tetrapentyl-2,20:3,19-dimetheno-
1H,21H,23H,25H-bis[1,3]dioxocino[5,4-i:5',4'-i']benzo[1,2-d:5,4-d']bis[1,3]
benzodioxocine stereoisomer
;
_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                93.6550(10)
_cell_angle_beta                 92.9210(10)
_cell_angle_gamma                118.6760(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5151(2)
_cell_length_b                   11.9323(2)
_cell_length_c                   22.7986(5)
_cell_measurement_reflns_used    7203
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.29
_cell_volume                     2730.83(9)
_computing_cell_refinement       'SAINT-NT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-NT (Bruker, 2005)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997) and
Mercury (Version 1.4.2; Bruno <i>et al.</i>,  2002)
;
_computing_publication_material  'SHELXTL (Bruker, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Bruker, 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42983
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         0.90
_exptl_absorpt_coefficient_mu    3.000
_exptl_absorpt_correction_T_max  0.4766
_exptl_absorpt_correction_T_min  0.3726
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
[face-indexed absorption corrections carried out with XPREP (Bruker,
2005)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_meas      1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1224.3
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.413
_refine_diff_density_min         -1.411
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         10730
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.113P)^2^+1.1716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1753
_refine_ls_wR_factor_ref         0.1873
_reflns_number_gt                7721
_reflns_number_total             10730
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2300.cif
_cod_data_source_block           I
_cod_database_code               2215973
_cod_database_fobs_code          2215973
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-03-21
;