Permanent Microporosity and Enantioselective Sorption in a Chiral Open Framework
Darren Bradshaw; Timothy J. Prior; Edmund J. Cussen; John B. Claridge; Matthew J. Rosseinsky; Journal of the American Chemical Society 126 (2004) 6106–6114; doi:10.1021/ja0316420

data_4112556
_publ_section_title
;
 Permanent Microporosity and Enantioselective Sorption in a Chiral Open
 Framework
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6106
_journal_page_last               6114
_journal_paper_doi               10.1021/ja0316420
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C63 H72 N6 Ni3 O18'
_chemical_formula_weight         1377.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           214
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I 4bd 2c 3'
_symmetry_space_group_name_H-M   'I 41 3 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.1350(4)
_cell_length_b                   28.1350(4)
_cell_length_c                   28.1350(4)
_cell_measurement_reflns_used    22506
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      46.93
_cell_measurement_theta_min      4.85
_cell_volume                     22271.1(5)
_computing_cell_refinement       'Bruker SAINT v.6.28a (Bruker, 2001)'
_computing_data_collection       'Bruker SMART v.5.054 (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT v.6.28a (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS SMART 1K CCD diffractometer'
_diffrn_measurement_method       'omega rotation with narrow frames'
_diffrn_radiation_monochromator  'Silicon 1 1 1'
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68750
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            56866
_diffrn_reflns_theta_full        23.84
_diffrn_reflns_theta_max         23.84
_diffrn_reflns_theta_min         1.98
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.9577
_exptl_absorpt_correction_T_min  0.9227
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.822
_exptl_crystal_description       block
_exptl_crystal_F_000             5760
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         3178
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.257
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0706
_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^)+(0.1746P)^2^+2.4173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2246
_refine_ls_wR_factor_ref         0.2366
_reflns_number_gt                2934
_reflns_number_total             3178
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0316420si20040301_103018_2.cif
_cod_data_source_block           desolvated_[Ni3(btc)2(3-pic)6(1,2-pd)3]
_cod_database_code               4112556