Incorporation of active metal sites in MOFs via in situ generated ligand deficient metal-linker complexes
Samir Barman; Hiroyasu Furukawa; Olivier Blacque; Koushik Venkatesan; Omar M. Yaghi; Guo-Xin Jin; Heinz Berke; Chem.Commun. 47 (2011) 11882–; doi:10.1039/c1cc14387e

data_7106988
_publ_section_title
;
 Incorporation of active metal sites in MOFs via in situ generated ligand
 deficient metal-linker complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              11882
_journal_paper_doi               10.1039/c1cc14387e
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C67 H71 Cu12 N25 O41, 2(C3 H7 N O), 2(O)'
_chemical_formula_sum            'C73 H85 Cu12 N27 O45'
_chemical_formula_weight         2823.28
_chemical_name_systematic
;
?
;
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c 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            2
_cell_length_a                   15.3345(1)
_cell_length_b                   14.5465(1)
_cell_length_c                   26.2229(3)
_cell_measurement_reflns_used    26187
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.7325
_cell_measurement_theta_min      2.3252
_cell_volume                     5849.37(9)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_molecular_graphics
; ORTEP-3 for Windows, Version 2.01.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
;
_computing_publication_material
; WinGX -- An integrated system of Windows programs for the solution,
refinment and analysis of single crystal X-ray diffraction data,
Version 1.80.00.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
SHELXL97. Program for crystal structure refinement.
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
PLATON for Windows, Version 1.12.
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.
;
_computing_structure_refinement
; SHELXL97. Program for crystal structure refinement.
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_solution
; SHELXS97. Program for Crystal Structure solution.
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
;
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
; Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            87527
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.48
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  90
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.224
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_correction_T_min  0.591
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.375
_refine_diff_density_min         -2.413
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         9101
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1162P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1820
_reflns_number_gt                6196
_reflns_number_total             9101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc14387e.txt
_cod_data_source_block           MOF-648
_cod_database_code               7106988