Ni(salphen)-based metal‒organic framework for the synthesis of cyclic carbonates by cycloaddition of CO2 to epoxides
Ren, Yanwei; Shi, Yanchao; Chen, Junxian; Yang, Shaorong; Qi, Chaorong; Jiang, Huanfeng; RSC Advances 3 (2013) 2167–; doi:10.1039/c2ra22550f

data_7238781
_publ_section_title
;
 Ni(salphen)-based metal--organic framework for the synthesis of cyclic
 carbonates by cycloaddition of CO2 to epoxides
;
_journal_issue                   7
_journal_name_full               'RSC Advances'
_journal_page_first              2167
_journal_paper_doi               10.1039/c2ra22550f
_journal_volume                  3
_journal_year                    2013
_chemical_formula_sum            'C77 H93 Cd2 N7 Ni2 O19'
_chemical_formula_weight         1762.81
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                89.29(3)
_cell_angle_beta                 87.12(3)
_cell_angle_gamma                68.48(3)
_cell_formula_units_Z            2
_cell_length_a                   16.348(3)
_cell_length_b                   16.635(3)
_cell_length_c                   20.293(4)
_cell_measurement_temperature    293(2)
_cell_volume                     5127(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0831
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38898
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  0.8538
_exptl_absorpt_correction_T_min  0.8538
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
Based on 236 electrons removed from the unit-cell
contents, this then corresponds with the removal of
236/2= 118 electrons from the asymmetric unit. as a DMF
molecule has 40 electrons, this might correspond
with the reomval of118/40 = 3 DMF molecules per asymmetric
unit so that the overall formula should then appear with
3 DMF of solvation as [Cd~2~(Ni-L)~2~(H~2~O)~4~].3DMF.
The contribution of disordered DMF solvent removed by
the SQUEEZE process has been included in the overall
formula, formula weight, density, F(000),etc..
Calculations were reported in ESI table S1
and in the CIF.
;
_refine_diff_density_max         1.001
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.0029(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         17511
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.0810
_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^)+(0.1408P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2369
_refine_ls_wR_factor_ref         0.2650
_reflns_number_gt                7378
_reflns_number_total             17511
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ra22550f.txt
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        5127.4(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7238781