Spontaneous chiral resolution of a 3D (3,12)-connected MOF with an unprecedented ttt topology consisting of cubic [Cd4(μ3-OH)4] clusters and propeller-like ligands
Yuan, Shuai; Deng, Yong-Kai; Xuan, Wei-Min; Wang, Xing-Po; Wang, Su-Na; Dou, Jian-Min; Sun, Di; CrystEngComm 16 (2014) 3829–; doi:10.1039/c4ce00028e

data_7214439
_publ_section_title
;
 Spontaneous chiral resolution of a 3D (3,12)-connected MOF with an
 unprecedented ttt topology consisting of cubic [Cd4(\m3-OH)4] clusters
 and propeller-like ligands
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              3829
_journal_paper_doi               10.1039/c4ce00028e
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C27 H22 Cd N7 O,NO3,C2H6O,C3H7NO'
_chemical_formula_sum            'C32 H35 Cd N9 O6'
_chemical_formula_weight         754.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           196
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'F 2 2 3'
_symmetry_space_group_name_H-M   'F 2 3'
_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            16
_cell_length_a                   25.3961(9)
_cell_length_b                   25.3961(9)
_cell_length_c                   25.3961(9)
_cell_measurement_reflns_used    1888
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      15.46
_cell_measurement_theta_min      2.27
_cell_volume                     16379.5(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0810
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            18992
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_T_max  0.9550
_exptl_absorpt_correction_T_min  0.9180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6176
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
Complex 1 has unusually large voids. 
The voids in the framework are filled with many disordered solvent
molecules and anions, which can not be located. Hence reflect on a high R(int)
value. In the refinement we used SQEEZE procedure 
(Spek, A.L. (2008) Utrecht University, Utrecht, 
The Netherlands) to remove solvent electron
density from voids which give a smaller final R(int) and R-value compared
with the original R(int) and R-value.
A main residual electron density of 1595 electrons/cell in cell-remaining voids 
where the residual electron density was tentatively assigned to 
1 NO3-, 1 EtOH and 1 DMF molecules [1595/16 = 99 for per formula of 1; 
98 = 40 (DMF) + 26 (EtOH) + 32 (NO3-)]. The numbers of and EtOH and 
DMF were also proved by the TGA and EA.
;
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.08(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.809
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2412
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0689
_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^)+(0.1700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1884
_refine_ls_wR_factor_ref         0.2091
_reflns_number_gt                1497
_reflns_number_total             2412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00028e2.cif
_cod_data_source_block           p-delta
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'F23  '
_cod_database_code               7214439