Construction of Two 3D Homochiral Frameworks with 1D Chiral Pores via Chiral Recognition
Huan-Yong Li; Long Jiang; Hua Xiang; Trevor A. Makal; Hong-Cai Zhou; Tong-Bu Lu; Inorganic Chemistry 50 (2011) 3177–3179; doi:10.1021/ic200264s

data_4324924
_publ_section_title
;
 Construction of Two 3D Homochiral Frameworks with 1D Chiral Pores via
 Chiral Recognition
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3177
_journal_page_last               3179
_journal_paper_doi               10.1021/ic200264s
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_sum            'C42 H90 Cl2 N10 Ni2 O12 S2'
_chemical_formula_weight         1179.68
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   19.0525(17)
_cell_length_b                   19.0525(17)
_cell_length_c                   18.1522(15)
_cell_measurement_reflns_used    2735
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.82
_cell_measurement_theta_min      2.91
_cell_volume                     5706.4(9)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 16.0855
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Gemini S Ultra'
_diffrn_measurement_method       '\w and \p scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1247
_diffrn_reflns_av_sigmaI/netI    0.1297
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13032
_diffrn_reflns_theta_full        59.99
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         3.62
_exptl_absorpt_coefficient_mu    2.163
_exptl_absorpt_correction_T_max  0.5181
_exptl_absorpt_correction_T_min  0.4782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.030
_exptl_crystal_description       block
_exptl_crystal_F_000             1890
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.35
_platon_squeeze_details
;

 of two types solvent from the data of TG, CHN analysis and crystal structure
due to vulnerable to loss of solvent molecules in this complex.

;
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         5042
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.1426
_refine_ls_R_factor_gt           0.0894
_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^)+(0.0853P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2024
_refine_ls_wR_factor_ref         0.2183
_reflns_number_gt                2128
_reflns_number_total             5042
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200264s_si_002.cif
_cod_data_source_block           delta-1
_cod_database_code               4324924