The synthesis and single crystal structure of an amino acid intercalated layered niobium phosphate: [(NbOPO4)4•(H3NCH2CO2H)2][H2PO4][OH, F]
Wang, Xiqu; Liu, Lumei; Cheng, Heidi; Jacobson, Allan J.; Chemical Communications  (1999) 2531–; doi:10.1039/a907293d

data_7110712
_publ_contact_author
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      Allan J. Jacobson
      Department of Chemistry
      University of Houston
      Houston, TX 77204-5641
      phone: 713-7432785
    E-mail:ajjacob@uh.edu
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_publ_section_title
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 The synthesis and single crystal structure of an amino acid intercalated
 layered niobium phosphate: [(NbOPO4)4&#x2022;(H3NCH2CO2H)2][H2PO4][OH, F]
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2531
_journal_paper_doi               10.1039/a907293d
_journal_year                    1999
_chemical_compound_source        'hydrothermal synthesis'
_chemical_formula_structural     '[NbOPO4]4.(H3NCH2COOH)2(H2PO4)(OH,F)'
_chemical_formula_sum            'C4 H14.6 F0.4 N2 Nb4 O28.6 P5'
_chemical_formula_weight         1082.3
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   ignored
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 109.304(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   17.020(2)
_cell_length_b                   6.4973(7)
_cell_length_c                   6.4992(7)
_cell_measurement_temperature    223(2)
_cell_volume                     678.30(13)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2117
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    1.988
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.650
_exptl_crystal_description       plate
_exptl_crystal_F_000             475
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.194
_refine_ls_extinction_coef       0.0032(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_all   1.173
_refine_ls_goodness_of_fit_obs   1.189
_refine_ls_hydrogen_treatment    ignored
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         850
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.172
_refine_ls_restrained_S_obs      1.188
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_obs          0.0345
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+7.1436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0892
_refine_ls_wR_factor_obs         0.0883
_reflns_number_observed          814
_reflns_number_total             850
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            907293dsup1.cif
_cod_data_source_block           '[NbOPO4]4'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+7.1436P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+7.1436P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        678.30(12)
_cod_original_sg_symbol_H-M      C2/m
_cod_original_formula_sum        'C4 N2 H14.6 O28.6 F0.4 Nb4 P5'
_cod_database_code               7110712