Nonaqueous Synthesis and Characterization of a Novel Layered Zirconium Phosphate Templated with Mixed Organic and Inorganic Cations
Wang, Dan; Yu, Ranbo; Kumada, Nobuhiro; Kinomura, Nobukazu; Chemistry of Materials 12 (2000) 956–960; doi:10.1021/cm990454z

data_4000028
_publ_section_title
;
 Nonaqueous Synthesis and Characterization of a Novel Layered Zirconium
 Phosphate Templated with Mixed Organic and Inorganic Cations
;
_journal_coden_ASTM              CMATEX
_journal_issue                   4
_journal_name_full               'Chemistry of Materials'
_journal_page_first              956
_journal_page_last               960
_journal_paper_doi               10.1021/cm990454z
_journal_volume                  12
_journal_year                    2000
_chemical_formula_moiety         'C4 H68 N6 O22 P4 Zr3 '
_chemical_formula_structural     (NH4)2[H3NCH2CH2NH3]2[Zr3(OH)6(PO4)4]
_chemical_formula_sum            'C4 H68 N6 O22 P4 Zr3'
_chemical_formula_weight         950.16
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Sun Jul 18 09:44:42 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                97.85(2)
_cell_angle_beta                 111.75(2)
_cell_angle_gamma                113.01(2)
_cell_formula_units_Z            1
_cell_length_a                   9.383(3)
_cell_length_b                   9.923(3)
_cell_length_c                   8.342(2)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      14.5
_cell_measurement_theta_min      10.3
_cell_volume                     627.0(5)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SAPI91
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.06251
_diffrn_orient_matrix_UB_12      0.08037
_diffrn_orient_matrix_UB_13      0.12319
_diffrn_orient_matrix_UB_21      -0.02863
_diffrn_orient_matrix_UB_22      -0.08356
_diffrn_orient_matrix_UB_23      0.05577
_diffrn_orient_matrix_UB_31      0.11125
_diffrn_orient_matrix_UB_32      -0.00127
_diffrn_orient_matrix_UB_33      0.01983
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_av_sigmaI/netI    0.191
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10755
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         45.02
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        0.51
_diffrn_standards_interval_count 500
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    15.6
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.425
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             980.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.27
_refine_ls_extinction_coef       0.0077(8)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_all   1.317
_refine_ls_goodness_of_fit_obs   1.632
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     179
_refine_ls_number_reflns         4242
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2028
_refine_ls_R_factor_obs          0.0511
_refine_ls_shift/esd_max         0.0670
_refine_ls_shift/esd_mean        0.0050
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'w = 1/[\s^2^(Fo) + 0.00004|Fo|^2^]'
_refine_ls_wR_factor_all         0.0717
_refine_ls_wR_factor_obs         0.0563
_reflns_number_observed          4242
_reflns_number_total             10337
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            cm990454z.cif
_cod_data_source_block           (NH4)2[H3NCH2CH2NH3]2[Zr3(OH)6(PO4)4]
_cod_original_formula_sum        'C4 H68 N6 O22 P4 Zr3 '
_cod_database_code               4000028