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_7214440
_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                   25.704(3)
_cell_length_b                   25.704(3)
_cell_length_c                   25.704(3)
_cell_measurement_reflns_used    585
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      4.25
_cell_volume                     16983(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0826
_diffrn_reflns_av_sigmaI/netI    0.0864
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            10189
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_T_max  0.9461
_exptl_absorpt_correction_T_min  0.9359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6176
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_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         0.514
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.836
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.836
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1337
_reflns_number_gt                1364
_reflns_number_total             2402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00028e2.cif
_cod_data_source_block           p-Lambda
_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.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' 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.

'_refine_ls_hydrogen_treatment' value 'CONSTR' changed
to 'constr' 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               7214440