The first porphyrin-salen based chiral metal-organic framework for asymmetric cyanosilylation of aldehydes
Jiang, Huanfeng; Li, Jiawei; Ren, Yanwei; Qi, Chaorong; Chem. Commun.  (2017) –; doi:10.1039/C7CC03499G

data_7120347
_publ_section_title
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 The first porphyrin-salen based chiral metal-organic framework for
 asymmetric cyanosilylation of aldehydes
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_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC03499G
_journal_year                    2017
_chemical_formula_sum            'C211 H200 Cd5 N22 Ni2 O31'
_chemical_formula_weight         4219.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-05-03 deposited with the CCDC.
2017-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                85.324(2)
_cell_angle_beta                 78.917(3)
_cell_angle_gamma                89.496(2)
_cell_formula_units_Z            1
_cell_length_a                   16.3993(4)
_cell_length_b                   17.3042(3)
_cell_length_c                   24.3278(10)
_cell_measurement_reflns_used    11487
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.9940
_cell_measurement_theta_min      2.7250
_cell_volume                     6752.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0909
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28338
_diffrn_reflns_theta_full        66.47
_diffrn_reflns_theta_max         66.47
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    3.597
_exptl_absorpt_correction_T_max  0.7150
_exptl_absorpt_correction_T_min  0.5332
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2159
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Based on 325 electrons removed from the unit-cell
contents, this then corresponds with the removle of 
325/1 = 325 electrons from the asymmetric unit. As a
DMF molecule has 40 electrons and a MeOH molecule has 
18 electrons, this might correspond with the removal of 
6 DMF molecules and 5 MeOH molecules per asymmetric
unit.This formula was also confirmed 
by elemental analysis and thermogravimetric analysis. 
The contribution of disordered DMF and 
MeOH 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 S1 and in the CIF. 
;
_refine_diff_density_max         5.877
_refine_diff_density_min         -3.087
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1938
_refine_ls_number_reflns         28338
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.1026
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1627P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2682
_refine_ls_wR_factor_ref         0.2951
_reflns_number_gt                17439
_reflns_number_total             28338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc03499g2.cif
_cod_data_source_block           li-sr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/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 4973 2017-02-22 13:04:09Z antanas 
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_cod_original_cell_volume        6752.2(3)
_cod_original_sg_symbol_H-M      P1
_cod_database_code               7120347