Design, Synthesis, Characterization, and Catalytic Properties of a Large-Pore Metal-Organic Framework Possessing Single-Site Vanadyl(monocatecholate) Moieties
Nguyen, Huong Giang T.; Weston, Mitchell H.; Sarjeant, Amy A.; Gardner, Daniel M.; An, Zhi; Carmieli, Raanan; Wasielewski, Michael R.; Farha, Omar K.; Hupp, Joseph T.; Nguyen, SonBinh T.; Crystal Growth & Design 13 (2013) 3528–; doi:10.1021/cg400500t

data_4507949
_publ_section_title
;
 Design, Synthesis, Characterization, and Catalytic Properties of a
 Large-Pore Metal-Organic Framework Possessing Single-Site
 Vanadyl(monocatecholate) Moieties
;
_journal_issue                   8
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3528
_journal_paper_doi               10.1021/cg400500t
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         'C56 H30 Br2 N2 O10 Zn2'
_chemical_formula_sum            'C56 H30 Br2 N2 O10 Zn2'
_chemical_formula_weight         1181.38
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           47
_space_group_name_Hall           '-P 2 2'
_space_group_name_H-M_alt        'P m m m'
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-03-20
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   11.4439(7)
_cell_length_b                   15.7580(9)
_cell_length_c                   23.466(2)
_cell_measurement_reflns_used    6393
_cell_measurement_temperature    225(2)
_cell_measurement_theta_max      58.57
_cell_measurement_theta_min      3.38
_cell_volume                     4231.7(5)
_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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XM, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      225.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1011
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17654
_diffrn_reflns_theta_full        60.48
_diffrn_reflns_theta_max         60.48
_diffrn_reflns_theta_min         1.88
_diffrn_source                   microsource
_diffrn_source_current           0.65
_diffrn_source_power             0.02925
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.1061 before and 0.0755 after correction.
The Ratio of minimum to maximum transmission is 0.7660.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.056
_refine_diff_density_max         3.890
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         3471
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0958
_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^)+(0.1975P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2657
_refine_ls_wR_factor_ref         0.2801
_reflns_number_gt                2277
_reflns_number_total             3471
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400500t_si_003.cif
_cod_data_source_block           n1694
_cod_database_code               4507949
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  Only the
atoms used in the refinement model are reported in the formula here.

Total solvent accessible volume / cell = 3305.0 Ang^3^ [78.1%]
Total electron count / cell = 1045.4
;