6,7-Bis(bromomethyl)-2,11,18,21,24,27-hexaoxatetracyclo[26.4.0.0^4,9^.0^12,17^]dotriaconta-1(28),4,6,8,12(17),13,15,29,31-nonaene dichloromethane monosolvate
Beack, Hyun Jin; Yoo, Seung Mee; Kim, Jae Eun; Sim, Wonbo; Lee, Jai Young; Acta Crystallographica Section E 68 (2012) o720–; doi:10.1107/S160053681200565X

data_2233938
_publ_section_title
;
 6,7-Bis(bromomethyl)-2,11,18,21,24,27-hexaoxatetracyclo[26.4.0.0^4,9^.0^12,17^]dotriaconta-1(28),4,6,8,12(17),13,15,29,31-nonaene
 dichloromethane monosolvate
;
_journal_coeditor_code           LX2226
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o720
_journal_paper_doi               10.1107/S160053681200565X
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C28 H30 Br2 O6, C H2 Cl2'
_chemical_formula_moiety         'C28 H30 Br2 O6, C H2 Cl2'
_chemical_formula_sum            'C29 H32 Br2 Cl2 O6'
_chemical_formula_weight         707.27
_chemical_name_systematic
;
6,7-Bis(bromomethyl)-2,11,18,21,24,27-
hexaoxatetracyclo[26.4.0.0^4,9^.0^12,17^]dotriaconta-
1(28),4,6,8,12(17),13,15,29,31-nonaene dichloromethane
monosolvate
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                66.116(7)
_cell_angle_beta                 85.263(9)
_cell_angle_gamma                77.080(6)
_cell_formula_units_Z            2
_cell_length_a                   9.133(3)
_cell_length_b                   12.191(4)
_cell_length_c                   15.038(6)
_cell_measurement_reflns_used    2021
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.06
_cell_measurement_theta_min      2.29
_cell_volume                     1492.1(9)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\p and \w 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  0.0497
_diffrn_reflns_av_sigmaI/netI    0.1272
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11188
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.936
_exptl_absorpt_correction_T_max  0.663
_exptl_absorpt_correction_T_min  0.575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.991
_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     352
_refine_ls_number_reflns         7310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1842
_refine_ls_R_factor_gt           0.0789
_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^)+(0.0893P)^2^+2.2498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1681
_refine_ls_wR_factor_ref         0.2427
_reflns_number_gt                3257
_reflns_number_total             7310
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lx2226.cif
_cod_data_source_block           I
_cod_original_cell_volume        1492.1(8)
_cod_database_code               2233938
_cod_database_fobs_code          2233938