Investigation of Porous Ni-Based Metal-Organic Frameworks Containing Paddle-Wheel Type Inorganic Building Units via High-Throughput Methods
Palanikumar Maniam; Norbert Stock; Inorganic Chemistry 50 (2011) 5085–5097; doi:10.1021/ic200381f

data_4325233
_publ_contact_author_address
;Institut fuer Anorganische Chemie, Universitaet Kiel,
Max-Eyth-Strasse 2, 24118 Kiel, Germany
;
_publ_contact_author_email       stock@ac.un-kiel.de
_publ_contact_author_fax         49(431)8801775
_publ_contact_author_name        'Prof. Dr. Norbert Stock'
_publ_contact_author_phone       49(431)8801675
_publ_section_title
;
 Investigation of Porous Ni-Based Metal-Organic Frameworks Containing
 Paddle-Wheel Type Inorganic Building Units via High-Throughput Methods
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5085
_journal_page_last               5097
_journal_paper_doi               10.1021/ic200381f
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C8 H9 N Ni O4'
_chemical_formula_weight         241.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           225
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 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            48
_cell_length_a                   26.5941(7)
_cell_length_b                   26.5941(7)
_cell_length_c                   26.5941(7)
_cell_measurement_reflns_used    43034
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.215
_cell_measurement_theta_min      1.325
_cell_volume                     18808.6(9)
_computing_cell_refinement       'X-Area (Stoe, 2008)'
_computing_data_collection       'X-Area (Stoe, 2008)'
_computing_data_reduction        'X-Area (Stoe, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       'Phi 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  0.0538
_diffrn_reflns_av_sigmaI/netI    0.0095
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            42290
_diffrn_reflns_theta_full        26.87
_diffrn_reflns_theta_max         26.87
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    1.229
_exptl_absorpt_correction_T_max  0.8967
_exptl_absorpt_correction_T_min  0.7674
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE XRED rev 1.19 and X-SHAPE rev 1.06'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             5952
_platon_squeeze_details
;
the highly disordered solvents within the void were not crystallographically
well defined.

The SQUEEZE routine of the program PLATON was used
in order to eliminate the contribution of disordered solvents molecules,
thereby a final model based only on the ordered part of the crystal structure
was obtained.

The SQUEEZE routine suggested that
a total potential solvent area volume of 10196.3 Ang^3^[54.2% of cell volume].

Refinement after the SQUEEZE routine gave significantly improved R values.
[R values before SQUEEZE]
R1 = 0.1144, wR2 = 0.4037 for >2sigma(I) data
R1 = 0.1161, wR2 = 0.4049, GooF = S = 1.962 for all data
( 1062 data and 0 restraint / 37 parameters)
;
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.286
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         1061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.286
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0676
_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^)+(0.0737P)^2^+99.1598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1800
_refine_ls_wR_factor_ref         0.1812
_reflns_number_gt                1031
_reflns_number_total             1061
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200381f_si_002.cif
_cod_data_source_block           1a
_cod_database_code               4325233