A General Thermolabile Protecting Group Strategy for Organocatalytic Metal-Organic Frameworks
David J. Lun; Geoffrey I. N. Waterhouse; Shane G. Telfer; Journal of the American Chemical Society 133 (2011) 5806–5809; doi:10.1021/ja202223d

data_4106006
_publ_section_title
;
 A General Thermolabile Protecting Group Strategy for Organocatalytic
 Metal-Organic Frameworks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5806
_journal_page_last               5809
_journal_paper_doi               10.1021/ja202223d
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C57 H48 N6 O16 Zn4'
_chemical_formula_weight         1334.49
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           215
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P -4 2 3'
_symmetry_space_group_name_H-M   'P -4 3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   17.160(3)
_cell_length_b                   17.160(3)
_cell_length_c                   17.160(3)
_cell_measurement_reflns_used    2371
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      50.0
_cell_measurement_theta_min      7.0
_cell_volume                     5053.0(15)
_computing_cell_refinement       'FSProcess in Process-Auto (Rigaku, 1998)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'FSProcess in Process-Auto (Rigaku, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      292(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Rigaku Spider'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  'Rigaku VariMax-HF Confocal Optical System'
_diffrn_radiation_source         'Rigaku MM007 rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3608
_diffrn_reflns_theta_full        32.11
_diffrn_reflns_theta_max         32.11
_diffrn_reflns_theta_min         7.30
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.439
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
The SQUEEZE routine indicated the presence of 225 residual electrons per unit 
cell, which corresponds to around 5 highly disordered DMF solvate molecules.  
Accounting for these solvate molecules in the final full matrix least squares 
refinement significantly improved the refinement statistics.
;
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.499
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         364
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.383
_refine_ls_R_factor_all          0.1317
_refine_ls_R_factor_gt           0.1286
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3200
_refine_ls_wR_factor_ref         0.3240
_reflns_number_gt                334
_reflns_number_total             364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja202223d_si_002_2.cif
_cod_data_source_block           IRMOF-Pro
_cod_database_code               4106006