Control of framework interpenetration for in situ modified hydroxyl functionalised IRMOFs
Damien Rankine; Antonio Avellaneda; Matthew R. Hill; Christian J. Doonan; Christopher J. Sumby; Chem.Commun. 48 (2012) 10328–; doi:10.1039/c2cc35565e

data_7108459
_publ_section_title
;
 Control of framework interpenetration for in situ modified hydroxyl
 functionalised IRMOFs
;
_journal_name_full               Chem.Commun.
_journal_page_first              10328
_journal_paper_doi               10.1039/c2cc35565e
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C52 H46 N2 O21 Zn4'
_chemical_formula_weight         1296.39
_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                   17.1227(14)
_cell_length_b                   17.1227(14)
_cell_length_c                   17.1227(14)
_cell_measurement_reflns_used    889
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.1158
_cell_measurement_theta_min      2.6589
_cell_volume                     5020.2(7)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1695
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_details
;
1 omega -68.00 -18.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- -16.3432 -77.0000 90.0000 50

;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_av_sigmaI/netI    0.1776
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4574
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.13
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
Application of the SQUEEZE routine resulted in significant
reductions in R1 and wR2 and an improvement in the GOF. R1,
wR2 and GOF before SQUEEZE routine: 17.12%, 44.44% and 1.203;
after SQUEEZE routine: 10.47%, 28.82% and 0.836. The contribution
of disordered solvent (114 electrons/unit cell) equates to 2
DEF solvent molecules which are included in the formula.
;
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.617
_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   0.19(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.832
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         1870
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.836
_refine_ls_R_factor_all          0.1875
_refine_ls_R_factor_gt           0.1047
_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^)+(0.1675P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2494
_refine_ls_wR_factor_ref         0.2882
_reflns_number_gt                744
_reflns_number_total             1870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35565e.txt
_cod_data_source_block           '[Zn4)(L1)3]'
_cod_original_sg_symbol_H-M      P-43m
_cod_database_code               7108459