Photolabile protecting groups in metal-organic frameworks: preventing interpenetration and masking functional groups
Rajesh K. Deshpande; Geoffrey I. N. Waterhouse; Geoffrey B. Jameson; Shane G. Telfer; Chem.Commun. 48 (2012) 1574–; doi:10.1039/c1cc12884a

data_7107258
_publ_section_title
;
 Photolabile protecting groups in metal-organic frameworks: preventing
 interpenetration and masking functional groups
;
_journal_name_full               Chem.Commun.
_journal_page_first              1574
_journal_paper_doi               10.1039/c1cc12884a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C63 H39 N3 O22 Zn4'
_chemical_formula_weight         1451.45
_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                   17.2108(17)
_cell_length_b                   17.2108(17)
_cell_length_c                   17.2108(17)
_cell_measurement_reflns_used    5863
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      71.8
_cell_measurement_theta_min      7.25
_cell_volume                     5098.0(9)
_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    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      292(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.902
_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  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21493
_diffrn_reflns_theta_full        64.94
_diffrn_reflns_theta_max         64.94
_diffrn_reflns_theta_min         7.28
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    0.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             734
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
SQUEEZE was used to account for the disordered solvent in the voids of
this MOF. The number of electrons corresponds to approximately 5 DEF
solvent molecules per unit cell. R1 was observed to drop from 0.247 to 0.121
and wR2 from 0.55 to 0.33.
;
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.6(2)
_refine_ls_extinction_coef       0.014(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.464
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         1535
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.462
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.1138
_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          0.3214
_refine_ls_wR_factor_ref         0.3304
_reflns_number_gt                1332
_reflns_number_total             1535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc12884a.txt
_cod_data_source_block           '[Zn4O(1)3]'
_cod_original_sg_symbol_H-M      P-43m
_cod_database_code               7107258