Post-Synthesis Alkoxide Formation Within Metal-Organic Framework Materials: A Strategy for Incorporating Highly Coordinatively Unsaturated Metal Ions
Karen L. Mulfort; Omar K. Farha; Charlotte L. Stern; Amy A. Sarjeant; Joseph T. Hupp; Journal of the American Chemical Society 131 (2009) 3866–3868; doi:10.1021/ja809954r

data_4104078
_publ_contact_author             'Joseph T. Hupp'
_publ_contact_author_email       j-hupp@northwestern.edu
_publ_section_title
;
 Post-Synthesis Alkoxide Formation Within Metal-Organic Framework
 Materials: A Strategy for Incorporating Highly Coordinatively Unsaturated
 Metal Ions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3866
_journal_page_last               3868
_journal_paper_doi               10.1021/ja809954r
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C65 H113 N15 O19 Zn'
_chemical_formula_weight         1474.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           47
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2'
_symmetry_space_group_name_H-M   'P m m 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                   11.3014(11)
_cell_length_b                   15.7553(13)
_cell_length_c                   15.7553(13)
_cell_measurement_reflns_used    7561
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.68
_cell_measurement_theta_min      2.56
_cell_volume                     2805.3(4)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2266
_diffrn_reflns_av_sigmaI/netI    0.2180
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34732
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.01
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.443
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.067
_platon_squeeze_details          ' ?'
_refine_diff_density_max         2.546
_refine_diff_density_min         -1.602
_refine_diff_density_rms         0.281
_refine_ls_extinction_coef       0.070(9)
_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   0.793
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         4765
_refine_ls_number_restraints     155
_refine_ls_restrained_S_all      0.826
_refine_ls_R_factor_all          0.1477
_refine_ls_R_factor_gt           0.1078
_refine_ls_shift/su_max          0.276
_refine_ls_shift/su_mean         0.022
_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          0.2575
_refine_ls_wR_factor_ref         0.2723
_reflns_number_gt                2290
_reflns_number_total             4765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809954r_si_002.cif
_cod_data_source_block           compound5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4104078