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_4507948
_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         'C61 H33 Br2 N2 O14 Zn2'
_chemical_formula_sum            'C61 H33 Br2 N2 O14 Zn2'
_chemical_formula_weight         1308.45
_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             2012-04-18
_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                   10.9619(11)
_cell_length_b                   16.0098(14)
_cell_length_c                   23.383(4)
_cell_measurement_reflns_used    2829
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.15
_cell_measurement_theta_min      4.03
_cell_volume                     4103.7(9)
_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      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_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  0.1381
_diffrn_reflns_av_unetI/netI     0.1017
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12093
_diffrn_reflns_theta_full        50.43
_diffrn_reflns_theta_max         50.43
_diffrn_reflns_theta_min         3.35
_diffrn_source                   microsource
_diffrn_source_current           0.65
_diffrn_source_power             0.02925
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.128
_exptl_absorpt_correction_T_max  0.7515
_exptl_absorpt_correction_T_min  0.4598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.1051 before and 0.0729 after correction.
The Ratio of minimum to maximum transmission is 0.6118.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             655
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.486
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2382
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.1584
_refine_ls_R_factor_gt           0.1208
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3308
_refine_ls_wR_factor_ref         0.3582
_reflns_number_gt                1272
_reflns_number_total             2382
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400500t_si_002.cif
_cod_data_source_block           n1639b
_cod_database_code               4507948
_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 = 2927.6 Ang^3^ [71.3%]
Total electron count / cell = 192.4
;