Two homochiral organocatalytic metal organic materials with nanoscopic channels
Zhuxiu Zhang; Young Ran Ji; Lukasz Wojtas; Wen-Yang Gao; Shengqian Ma; Michael J. Zaworotko; Jon C. Antilla; Chem.Commun. 49 (2013) 7693–; doi:10.1039/c3cc43801e

data_7109657
_publ_section_title
;
 Two homochiral organocatalytic metal organic materials with nanoscopic
 channels
;
_journal_name_full               Chem.Commun.
_journal_page_first              7693
_journal_paper_doi               10.1039/c3cc43801e
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C52 H19 Cd2 O20 P'
_chemical_formula_weight         1219.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   17.4396(10)
_cell_length_b                   22.4040(15)
_cell_length_c                   29.2728(18)
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      64.37
_cell_measurement_theta_min      3.16
_cell_volume                     11437.4(12)
_computing_cell_refinement       'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)'
_computing_publication_material  'APEX2 (Bruker, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'BRUKER SMART APEXII CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            96572
_diffrn_reflns_theta_full        64.74
_diffrn_reflns_theta_max         64.74
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    3.415
_exptl_absorpt_correction_T_max  0.8250
_exptl_absorpt_correction_T_min  0.8250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.708
_exptl_crystal_density_meas      0.708
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;

the solvent molecules removed by the SQUEEZE process could be regarded 
as DMF molecules and dimethylammonium cations(DMA+) as counterions. 
In every single unit cell, there are 16 dimethylammonium cations containing 
416 electrons, so the rest of 2594 C 416 = 2178 electrons are belongs to DMF molecules. 
As a result, there are ~55 DMF molecules per unit cell. The theoretical occupied volume 
of single DMF molecule and dimethylammonium cations are 75.26  and 55.33  respectively, 
indicating total volume of free molecules is 75.26*54 + 55.33*16 = 5024.58  per unit cell 
which is much smaller than 7921 calculated by PLATON. 

;
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         19193
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0054P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0713
_reflns_number_gt                16705
_reflns_number_total             19193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc43801e.txt
_cod_data_source_block           ocMOM-2
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               7109657