A Chiral Salen-based MOF Catalytic Material with highly thermal, aqueous and chemical stabilities
Jiang, Huanfeng; jiawei, Li; Ren, Yanwei; Qi, Chaorong; Dalton Trans.  (2017) –; doi:10.1039/C7DT01116D

data_7043028
_publ_section_title
;
 A Chiral Salen-based MOF Catalytic Material with highly thermal, aqueous
 and chemical stabilities
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01116D
_journal_year                    2017
_chemical_formula_sum            'C250 H325 Cu8 I8 N39 Ni4 O28'
_chemical_formula_weight         6082.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2bc 2'
_space_group_name_H-M_alt        'P 2 21 21'
_symmetry_space_group_name_Hall  'P 2bc 2'
_symmetry_space_group_name_H-M   'P 2 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-04-27 deposited with the CCDC.
2017-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.42479(20)
_cell_length_b                   35.8993(7)
_cell_length_c                   36.7318(4)
_cell_measurement_reflns_used    20348
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.7980
_cell_measurement_theta_min      2.6740
_cell_volume                     24295.8(6)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            51325
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        66.207
_diffrn_reflns_theta_max         66.207
_diffrn_reflns_theta_min         1.721
_exptl_absorpt_coefficient_mu    9.389
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40328
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       block
_exptl_crystal_F_000             12357
_platon_squeeze_details
;
Based on 3461 electrons removed from the unit-cell
contents, this then corresponds with the removle of 
3461/4 = 866 electrons from the asymmetric unit. As a
DMF molecule has 40 electrons and a MeCN molecule has 
22 electrons, this might correspond with the removal of 
20 DMF molecules and 3 MeCN molecules per asymmetric
unit so that the overall formula should then appear with 
20 DMF and 3 MeCN of solvation as [(Cu~4~I~4~)~2~L~4~].
20DMF.3MeCN.In addition, this formula was also confirmed 
by elemental analysis, thermogravimetric analysis and 
HNMR studies. The contribution of disordered DMF and 
MeCN solvent molecules removed by the SQUEEZE process
has been included in the overall formula, formula weight,
densit, F(000), etc..Calculations were reported in
Table 1 and in the CIF. 
;
_refine_diff_density_max         3.620
_refine_diff_density_min         -3.755
_refine_diff_density_rms         0.242
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         35689
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1346
_refine_ls_R_factor_gt           0.1242
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1567P)^2^+584.9174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3141
_refine_ls_wR_factor_ref         0.3234
_reflns_Friedel_coverage         0.875
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                30079
_reflns_number_total             35689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01116d2.cif
_cod_data_source_block           ljw_16091109_sqd
_cod_database_code               7043028
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              63960
_platon_squeeze_void_probe_radius 1.20