Amide Functionalized Metal Organic Frameworks for Diastereoselective Nitroaldol (Henry) Reaction in Aqueous Medium
Paul, Anup; Karmakar, Anirban; Guedes da Silva, M. Fátima C.; Pombeiro, Armando J. L.; RSC Adv.  (2015) –; doi:10.1039/C5RA14637B

data_7222407
_publ_section_title
;
 Amide Functionalized Metal Organic Frameworks for Diastereoselective
 Nitroaldol (Henry) Reaction in Aqueous Medium
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA14637B
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C34 H22 N4 O10 Zn2, 2(C3 H7 N O)'
_chemical_formula_sum            'C40 H36 N6 O12 Zn2'
_chemical_formula_weight         923.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-09-17 deposited with the CCDC.
2015-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.560(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0350(9)
_cell_length_b                   24.892(3)
_cell_length_c                   10.8856(13)
_cell_measurement_reflns_used    9524
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.59
_cell_volume                     2024.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury CSD 3.5.1, 2008'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1999)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II PHOTON 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            46996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.372
_diffrn_reflns_theta_min         2.012
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       block
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.499(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         7404
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.6282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.952
_reflns_friedel_fraction_full    0.999
_reflns_friedel_fraction_max     0.998
_reflns_number_gt                7306
_reflns_number_total             7404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra14637b2.cif
_cod_data_source_block           Compound1
_cod_database_code               7222407
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.689
_shelx_estimated_absorpt_t_max   0.874
_shelx_res_checksum              39487