Synthesis, Structure Determination, and Hydrogen Sorption Studies of New Metal−Organic Frameworks Using Triazole and Naphthalenedicarboxylic Acid
Park, Hyunsoo; Britten, James F.; Mueller, Ulrich; Lee, JeongYong; Li, Jing; Parise, John B.; Chemistry of Materials 19 (2007) 1302–; doi:10.1021/cm0623918

data_4001301
_publ_section_title
;
 Synthesis, Structure Determination, and Hydrogen Sorption Studies of New
 Metal&#x2212;Organic Frameworks Using Triazole and
 Naphthalenedicarboxylic Acid
;
_journal_issue                   6
_journal_name_full               'Chemistry of Materials'
_journal_page_first              1302
_journal_paper_doi               10.1021/cm0623918
_journal_volume                  19
_journal_year                    2007
_chemical_formula_moiety         Zn4(C2H2N3)4(C12H6O4)2.(2C3H7ON).(4O)
_chemical_formula_sum            'C38 H34 N14 O14 Zn4'
_chemical_formula_weight         1172.27
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            4
_cell_length_a                   30.978(6)
_cell_length_b                   12.620(3)
_cell_length_c                   13.339(3)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.95
_cell_measurement_theta_min      1.41
_cell_volume                     5215(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Diamond 3.0'
_computing_publication_material  'SHELXTL (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2000)'
_computing_structure_solution    'SHELXS (Sheldrick, 2000)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  '4-circle goniometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.49594
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19004
_diffrn_reflns_theta_full        16.95
_diffrn_reflns_theta_max         16.95
_diffrn_reflns_theta_min         1.41
_diffrn_source                   synchrotron
_diffrn_source_type              'APS beamline 15-ID'
_exptl_absorpt_coefficient_mu    0.997
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2368
_exptl_crystal_recrystallization_method hydrothermal
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.382
_refine_diff_density_min         -1.909
_refine_diff_density_rms         0.413
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(18)
_refine_ls_extinction_coef       0.118(7)
_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   1.236
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         7114
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.236
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.1103
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1788P)^2^+16.1535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2743
_refine_ls_wR_factor_ref         0.2837
_reflns_number_gt                6766
_reflns_number_total             7114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm0623918si20061006_115210.cif
_cod_data_source_block           pna21
_cod_original_cell_volume        5215.0(18)
_cod_database_code               4001301