Preparation of solvent-free clathrand structures by the exclusion of an unwelcome guest
Bishop, Roger; Rahman, A. Noman M. M.; Ashmore, Jason; Craig, Donald C.; Scudder, Marcia L.; CrystEngComm 4 (2002) 605–; doi:10.1039/b210215c

data_7216567
_publ_section_title
;
 Preparation of solvent-free clathrand structures by the exclusion of an
 unwelcome guest
;
_journal_issue                   101
_journal_name_full               CrystEngComm
_journal_page_first              605
_journal_paper_doi               10.1039/b210215c
_journal_volume                  4
_journal_year                    2002
_chemical_formula_moiety         'C22 H12 Br4 N2'
_chemical_formula_sum            'C22 H12 Br4 N2'
_chemical_formula_weight         624.0
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_type_scat_source
'International Tables for X-ray Crystallography, Vol. IV'
_audit_creation_method           'RAELSPUB and manual entry'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.579(7)
_cell_length_b                   32.870(8)
_cell_length_c                   4.447(1)
_cell_measurement_reflns_used    10
_cell_measurement_temperature    294
_cell_measurement_theta_max      15
_cell_measurement_theta_min      13
_cell_volume                     4031.3(17)
_computing_cell_refinement       'CAD4 Version 5.0, 1989'
_computing_data_collection       'CAD4 Version 5.0, 1989'
_computing_data_reduction        'Local program'
_computing_molecular_graphics    'ORTEP-II, (Johnson, 1976)'
_computing_publication_material  'Local programs'
_computing_structure_refinement  'RAELS, (Rae, 1989)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1011
_diffrn_reflns_theta_max         25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  30min
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    7.919
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(DeMeulenaer & Tompa, 1965)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.06
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2384.0
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.02
_refine_diff_density_min         -0.68
_refine_ls_abs_structure_details
'The polarity is confirmed, the alternative giving R 0.042'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.69
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     67
_refine_ls_number_reflns         811
_refine_ls_R_factor_gt           0.039
_refine_ls_shift/su_max          0.005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F) + 0.0004F^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.048
_reflns_number_gt                811
_reflns_number_total             1011
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b210215c.txt
_cod_data_source_block           DRB254_C22H12Br4N2
_cod_original_cell_volume        4031(2)
_cod_database_code               7216567