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_4001300
_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).(3H2O)'
_chemical_formula_sum            'C38 H34 N14 O13 Zn4'
_chemical_formula_weight         1156.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 92.463(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.609(2)
_cell_length_b                   27.181(5)
_cell_length_c                   13.617(3)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      65.23
_cell_measurement_theta_min      3.25
_cell_volume                     5032.4(16)
_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 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.5741
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8494
_diffrn_reflns_theta_full        24.77
_diffrn_reflns_theta_max         24.77
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    1.955
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_correction_T_min  0.621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Shledrick, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.235
_refine_diff_density_min         -1.791
_refine_diff_density_rms         0.200
_refine_ls_extinction_coef       0.0035(4)
_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   0.942
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         8314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.2650
_refine_ls_R_factor_gt           0.1033
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1062P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2347
_refine_ls_wR_factor_ref         0.2742
_reflns_number_gt                2579
_reflns_number_total             8314
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm0623918si20061006_115210.cif
_cod_data_source_block           twin4
_cod_original_cell_volume        5032.6(16)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4001300