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_7108460
_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            'C97 H72.33 N0.33 O38.33 Zn8'
_chemical_formula_weight         2378.85
_chemical_name_systematic
;
?
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   23.5302(8)
_cell_length_b                   23.5302(8)
_cell_length_c                   31.5110(14)
_cell_measurement_reflns_used    12330
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.8533
_cell_measurement_theta_min      2.5908
_cell_volume                     15109.3(10)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_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 0.998
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details
;
1 omega -52.00 89.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 23.2851 -10.0000 -150.0000 141

2 omega -96.00 -44.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- -23.7539 -77.0000 30.0000 52

3 omega -90.00 52.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- -23.7539 19.0000 176.0000 142

;
_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  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            31783
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.91
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.979
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3610
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
In line with the treatment of [Zn4O(L1)3], the SQUEEZE routine
of PLATON was applied to the collected data, which resulted in
reductions in R1 and wR2 and an improvement in the GOF. R1, wR2
and GOF before SQUEEZE routine: 5.98%, 18.27% and 1.613; after
SQUEEZE routine: 4.76%, 12.79% and 1.121. The contribution of
disordered solvent (28 electrons/unit cell) equates to
approximately one DMF molecule per unit cell which was
included in the formula.
;
_refine_diff_density_max         1.902
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         4741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1279
_reflns_number_gt                3405
_reflns_number_total             4741
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35565e.txt
_cod_data_source_block           a-[Zn4O(L2)3]
_cod_original_sg_symbol_H-M      R-3m
_cod_database_code               7108460