Enhanced Gas Sorption Properties and Unique Behavior toward Liquid Water in a Pillared-Paddlewheel Metal-Organic Framework Transmetalated with Ni(II).
Karagiaridi, Olga; Bury, Wojciech; Fairen-Jimenez, David; Wilmer, Christopher E.; Sarjeant, Amy A.; Hupp, Joseph T.; Farha, Omar K.; Inorganic chemistry 53 (2014) 10432–10436; doi:10.1021/ic501467w

data_4341085
_publ_section_title
;
 Enhanced Gas Sorption Properties and Unique Behavior toward Liquid Water
 in a Pillared-Paddlewheel Metal-Organic Framework Transmetalated with
 Ni(II).
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10432
_journal_page_last               10436
_journal_paper_doi               10.1021/ic501467w
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C46 H38 N2 O8 Zn2'
_chemical_formula_sum            'C46 H38 N2 O8 Zn2'
_chemical_formula_weight         877.52
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           123
_space_group_name_Hall           '-P 4 2'
_space_group_name_H-M_alt        'P 4/m m m'
_symmetry_space_group_name_Hall  '-P 4 2'
_symmetry_space_group_name_H-M   'P 4/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-03-22
_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                   15.6918(3)
_cell_length_b                   15.6918(3)
_cell_length_c                   9.4600(3)
_cell_measurement_reflns_used    7751
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      61.47
_cell_measurement_theta_min      2.82
_cell_volume                     2329.36(10)
_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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0658
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12675
_diffrn_reflns_theta_full        61.68
_diffrn_reflns_theta_max         61.68
_diffrn_reflns_theta_min         2.82
_diffrn_source                   microsource
_diffrn_source_current           0.65
_diffrn_source_power             0.02925
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.838
_exptl_absorpt_correction_T_max  0.7520
_exptl_absorpt_correction_T_min  0.6186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.1034 before and 0.0733 after correction.
The Ratio of minimum to maximum transmission is 0.8226.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.583
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.766
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         1108
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.937
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.1169
_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          0.3485
_refine_ls_wR_factor_ref         0.3567
_reflns_number_gt                1003
_reflns_number_total             1108
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501467w_si_002.cif
_cod_data_source_block           n1559
_cod_depositor_comments          'Adding full bibliography for 4341085.cif.'
_cod_database_code               4341085
_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 = 1448.5 Ang^3^ [62.2%]
Total electron count / cell = 414.5
;