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_4112554
_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_structural
'Ni 3 (C 9 H 3 O 6) 2 (C 6 H 7 N) 6 (C 4 H 10 O)'
_chemical_formula_sum            'C60 H54 N6 Ni3 O18'
_chemical_formula_weight         1323.33
_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                   27.983(7)
_cell_length_b                   27.983(7)
_cell_length_c                   27.983(7)
_cell_measurement_reflns_used    6364
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.41
_cell_measurement_theta_min      3.01
_cell_volume                     21912(9)
_computing_cell_refinement       'LSCELL (Clegg, 1997)'
_computing_data_collection       'Bruker AXS SMART'
_computing_data_reduction        'Bruker AXS SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.499
_diffrn_measured_fraction_theta_max 0.499
_diffrn_measurement_device_type  'Bruker AXS SMART CCD diffractometer'
_diffrn_measurement_method       'omega rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.69310
_diffrn_reflns_av_R_equivalents  0.1134
_diffrn_reflns_av_sigmaI/netI    0.0883
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            20156
_diffrn_reflns_theta_full        25.79
_diffrn_reflns_theta_max         25.79
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M., SADABS; Universitat Gottingen, 1997'
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.802
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             5471
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         3780
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1729
_refine_ls_R_factor_gt           0.1123
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1993P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2889
_refine_ls_wR_factor_ref         0.3266
_reflns_number_gt                2237
_reflns_number_total             3780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0316420si20031210_095716.cif
_cod_data_source_block           Ni3(btc)2(3-picoline)6(C4H9OH)6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1993P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1993P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        21912(10)
_cod_database_code               4112554