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_7109656
_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_moiety
'[(C144 H72 O44 P3 In6) (NO3-)2 (C2H6O)106.67]  '
_chemical_formula_sum            'C357.33 H712 In6 N2 O156.67 P3'
_chemical_formula_weight         8325.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                   31.1023(19)
_cell_length_b                   31.1023(19)
_cell_length_c                   45.205(3)
_cell_measurement_temperature    100(2)
_cell_volume                     37871(4)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'BRUKER SMART APEXII CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0976
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            46316
_diffrn_reflns_theta_full        13.43
_diffrn_reflns_theta_max         13.43
_diffrn_reflns_theta_min         0.68
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.9713
_exptl_absorpt_correction_T_min  0.9713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             13387
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;

there is no significant amount of DMF molecules in the void of the structure or coordinated to metal atoms. 
The solvent molecules removed by the SQUEEZE process could be regarded as EtOH molecules as well as nitrate anions. 
In every single unit cell, there are 6 nitrate anions containing 186 electrons, so the rest of 8510 C 186 = 8324 
electrons are belongs to EtOH molecules. As a result, there are 320 EtOH molecules per unit cell. 
The theoretical occupied volume of single EtOH molecule and nitrate anion are 49.41and 38.61  respectively, 
indicating total volume of free molecules is 49.41*320 + 38.61*6 = 16042 per unit cell which is much smaller 
than 28926 calculated by PLATON. 

;
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.088(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1015
_refine_ls_number_reflns         23627
_refine_ls_number_restraints     380
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1120
_reflns_number_gt                15024
_reflns_number_total             23627
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc43801e.txt
_cod_data_source_block           ocMOM-1
_cod_original_cell_volume        37870(4)
_cod_original_sg_symbol_H-M      R3
_cod_database_code               7109656