Zinc metal-organic frameworks: efficient catalysts for the diastereoselective Henry reaction and transesterification.
Karmakar, Anirban; Guedes da Silva, M Fátima C; Pombeiro, Armando J. L.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 7795–7810; doi:10.1039/c4dt00219a

data_7029669
_publ_section_title
;
 Zinc metal-organic frameworks: efficient catalysts for the
 diastereoselective Henry reaction and transesterification.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7795
_journal_page_last               7810
_journal_paper_doi               10.1039/c4dt00219a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C39 H47 N5 O21 Zn4, 9(C4 H8 O2)'
_chemical_formula_sum            'C75 H119 N5 O39 Zn4'
_chemical_formula_weight         1976.22
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 103.171(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.4488(6)
_cell_length_b                   18.1141(7)
_cell_length_c                   17.5541(7)
_cell_measurement_reflns_used    4883
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.80
_cell_measurement_theta_min      2.55
_cell_volume                     4783.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0917
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
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_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33504
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.147
_diffrn_reflns_theta_min         2.292
_exptl_absorpt_coefficient_mu    1.076
_exptl_absorpt_correction_T_max  0.8059
_exptl_absorpt_correction_T_min  0.7262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       prism
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.320
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_platon_squeeze_details
;
 It was found that the disordered solvent is dioxane, with four independent
 molecules in general positions and one at a crystallographic inversion centre, 
 all of them disordered, so that the oxygen positions cannot be  ascertained.
 The asymmetric unit contains 4.5 molecules, hence there are 9  molecules per
 formula unit, and 18 per unit cell. This gives 884 electrons in
 all, not too far away from 772 electrons estimated by PLATON SQUEEZE. The
 refinement with (and without) various disorder models gives R1 between 8 and 9%. 
 Thus, the solvent-masking gives better results both considering R and the refinement
 of the host molecule. 
 The dioxane molecules were explicitly included into the CIF.
;
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         10561
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1005P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5565
_reflns_number_total             10561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt00219a2.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/usr/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 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7029668--7029670.cif.
;
_cod_database_code               7029669
_shelx_estimated_absorpt_t_min   0.733
_shelx_estimated_absorpt_t_max   0.812
_shelxl_version_number           2013-4
_shelx_res_checksum              5043