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_7222408
_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_formula_moiety         'C26 H18 Cu N4 O6, 4(C3 H7 N O), H2 O'
_chemical_formula_sum            'C38 H48 Cu N8 O11'
_chemical_formula_weight         856.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.700(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3259(14)
_cell_length_b                   22.773(4)
_cell_length_c                   20.105(3)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.22
_cell_volume                     3804.1(11)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.984
_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  0.1053
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_laue_measured_fraction_full 0.989
_diffrn_reflns_laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43898
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.501
_diffrn_reflns_theta_min         2.592
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       block
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_platon_squeeze_details
;
 The Platon SQUEEZE procedure was applied to recover 562 electrons per
 unit cell in a void (total volume 1266 A^3), that is, 141 electrons
 per formula unit. On the basis of microanalytical data, the void content
 may include 1 water and 3 dmf molecules, i.e., a total of 130 electrons not
 far from the values estimated by SQUEEZE. Those solvent molecules have
 been included in the formula for the calculation of intensive  properties,
 thus justifying the checkcif report allerts CHEMW03_ALERT_2_A and
 DIFF003_ALERT_1_A. 
 PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13.
;
_refine_diff_density_max         1.293
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         6972
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.0834
_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^)+(0.1135P)^2^+8.8555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2110
_refine_ls_wR_factor_ref         0.2268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4604
_reflns_number_total             6972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra14637b2.cif
_cod_data_source_block           Compound2
_cod_database_code               7222408
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.834
_shelx_estimated_absorpt_t_max   0.926
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              58827