Enantioselective Diels‒Alder reaction in confined space of homochiral metal‒organic frameworks
Tanaka, Koichi; Nagase, Shohei; Anami, Suguru; Wierzbicki, Michal; Urbanczyk-Lipkowska, Zofia; RSC Adv.  (2016) –; doi:10.1039/C6RA23740A

data_7227130
_publ_section_title
;
 Enantioselective Diels--Alder reaction in confined space of homochiral
 metal--organic frameworks
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA23740A
_journal_year                    2016
_chemical_absolute_configuration (R)
_chemical_formula_moiety         'MOF-1A+3DMF+MeOH+2-3 extra DMF'
_chemical_formula_sum            'C78 H64 Cu2 N3 O16'
_chemical_formula_weight         1426.43
_chemical_name_common            (R)-MOF-1A
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2'
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-06-03 deposited with the CCDC.
2016-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   33.835(5)
_cell_length_b                   33.835(5)
_cell_length_c                   39.859(8)
_cell_measurement_reflns_used    827
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      7.9182
_cell_measurement_theta_min      3.9497
_cell_volume                     39517(11)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'MXCuBE (Gabadinho, 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    Mercury
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.724
_diffrn_measured_fraction_theta_max 0.404
_diffrn_measurement_device_type  'MD2 instrument with a mini-kappa goniostat'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6888
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0158
_diffrn_reflns_Laue_measured_fraction_full 0.724
_diffrn_reflns_Laue_measured_fraction_max 0.404
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       59
_diffrn_reflns_limit_k_min       -59
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            137923
_diffrn_reflns_point_group_measured_fraction_full 0.714
_diffrn_reflns_point_group_measured_fraction_max 0.392
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.997
_diffrn_reflns_theta_min         0.862
_diffrn_source                   'P13 Beamline PETRA III Synchrotron'
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_density_meas      1.328
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prism
_exptl_crystal_F_000             13302
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.952
_exptl_transmission_factor_min   0.862
_refine_diff_density_max         1.619
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details
;
 Flack x determined using 7528 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
 
;
_refine_ls_abs_structure_Flack   0.055(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     953
_refine_ls_number_reflns         17540
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.584
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0732
_refine_ls_shift/su_max          2.607
_refine_ls_shift/su_mean         0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1845P)^2^+77.6029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2230
_refine_ls_wR_factor_ref         0.2263
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_full    0.703
_reflns_Friedel_fraction_max     0.380
_reflns_number_gt                25498
_reflns_number_total             49125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra23740a2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        39518(16)
_cod_database_code               7227130
_shelxl_version_number           2014/6
_shelx_res_checksum              16333