#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/90/7009009.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7009009
loop_
_publ_author_name
'Kongshaug, Kjell Ove'
'Fjellvag, Helmer'
'Lillerud, Karl Petter'
_publ_section_title
;
 The synthesis and crystal structure of UiO-19; an organically
 templated layered titanium phosphate with the ULM-11 topology
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              551
_journal_paper_doi               10.1039/a908051a
_journal_year                    2000
_chemical_formula_sum            'C2 H9 N2 O5 P Ti'
_chemical_formula_weight         219.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.6130(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2650(2)
_cell_length_b                   7.35460(10)
_cell_length_c                   9.91780(10)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      3.47
_cell_volume                     664.242(18)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART CCD'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       scanning
_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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9127
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    1.506
_exptl_absorpt_correction_type   'Empirical with SADABS'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    2.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platlet
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.035
_refine_diff_density_max         1.364
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0315
_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/[σ²(Fo²)+(0.0364P)²+1.0746P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                1810
_reflns_number_total             2015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a908051a.txt
_cod_data_source_block           UiO-19
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C2 H9 N2 O5 P1 Ti1'
_cod_database_code               7009009
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti Ti -0.00728(3) 0.14474(4) 0.23210(3) 0.00674(10) Uani 1 1 d . . .
P P -0.20843(5) 0.13204(6) -0.08662(4) 0.00494(11) Uani 1 1 d . . .
O1 O -0.37679(14) 0.12822(17) -0.12595(14) 0.0091(2) Uani 1 1 d . . .
O2 O -0.16764(15) 0.14574(18) 0.07053(13) 0.0096(3) Uani 1 1 d . . .
O3 O 0.14285(15) 0.04307(17) 0.13536(13) 0.0091(2) Uani 1 1 d . . .
O4 O -0.15139(14) 0.19685(17) 0.35027(13) 0.0084(2) Uani 1 1 d . . .
O5 O -0.05117(15) -0.13423(16) 0.27525(13) 0.0082(2) Uani 1 1 d . . .
N1 N 0.15071(18) 0.1009(2) 0.42651(16) 0.0099(3) Uani 1 1 d . . .
N2 N 0.50631(18) 0.2900(2) 0.62289(17) 0.0100(3) Uani 1 1 d . . .
C1 C 0.3836(2) 0.1556(2) 0.58807(19) 0.0095(3) Uani 1 1 d . . .
C2 C 0.2958(2) 0.1883(3) 0.44393(18) 0.0096(3) Uani 1 1 d . . .
H1 H 0.111(4) 0.137(4) 0.490(4) 0.030 Uiso 1 1 d . . .
H2 H 0.155(4) -0.011(5) 0.436(3) 0.030 Uiso 1 1 d . . .
H3 H 0.561(3) 0.262(5) 0.702(4) 0.030 Uiso 1 1 d . . .
H4 H 0.469(4) 0.395(4) 0.632(3) 0.030 Uiso 1 1 d . . .
H5 H 0.560(4) 0.294(4) 0.557(4) 0.030 Uiso 1 1 d . . .
H6 H 0.424(4) 0.034(5) 0.599(3) 0.030 Uiso 1 1 d . . .
H7 H 0.325(4) 0.169(4) 0.657(4) 0.030 Uiso 1 1 d . . .
H8 H 0.283(3) 0.317(5) 0.427(3) 0.030 Uiso 1 1 d . . .
H9 H 0.358(4) 0.143(4) 0.375(4) 0.030 Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Ti O4 95.43(6) 2 . ?
O5 Ti O2 99.09(6) 2 . ?
O4 Ti O2 89.48(6) . . ?
O5 Ti O3 94.69(6) 2 . ?
O4 Ti O3 167.77(5) . . ?
O2 Ti O3 95.69(6) . . ?
O5 Ti O5 169.55(2) 2 . ?
O4 Ti O5 83.88(5) . . ?
O2 Ti O5 91.34(5) . . ?
O3 Ti O5 84.92(5) . . ?
O5 Ti N1 90.67(6) 2 . ?
O4 Ti N1 85.54(6) . . ?
O2 Ti N1 169.44(6) . . ?
O3 Ti N1 87.49(6) . . ?
O5 Ti N1 78.88(6) . . ?
O1 P O2 107.87(8) . . ?
O1 P O3 110.24(7) . 3 ?
O2 P O3 109.60(7) . 3 ?
O1 P O4 108.65(7) . 4_565 ?
O2 P O4 108.62(7) . 4_565 ?
O3 P O4 111.77(7) 3 4_565 ?
P O2 Ti 146.09(9) . . ?
P O3 Ti 145.36(8) 3 . ?
P O4 Ti 136.14(8) 4_566 . ?
Ti O5 Ti 145.21(8) 2_545 . ?
C2 N1 Ti 118.73(11) . . ?
C2 N1 H1 107(2) . . ?
Ti N1 H1 107(2) . . ?
C2 N1 H2 113(2) . . ?
Ti N1 H2 105(2) . . ?
H1 N1 H2 104(3) . . ?
C1 N2 H3 110(2) . . ?
C1 N2 H4 108(2) . . ?
H3 N2 H4 108(3) . . ?
C1 N2 H5 111(2) . . ?
H3 N2 H5 110(3) . . ?
H4 N2 H5 110(3) . . ?
N2 C1 C2 111.23(15) . . ?
N2 C1 H6 109(2) . . ?
C2 C1 H6 112(2) . . ?
N2 C1 H7 106(2) . . ?
C2 C1 H7 113(2) . . ?
H6 C1 H7 106(3) . . ?
N1 C2 C1 111.00(14) . . ?
N1 C2 H8 108.9(19) . . ?
C1 C2 H8 110(2) . . ?
N1 C2 H9 113.2(19) . . ?
C1 C2 H9 107.6(19) . . ?
H8 C2 H9 106(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti O5 1.7192(12) 2 ?
Ti O4 1.9697(13) . ?
Ti O2 1.9745(13) . ?
Ti O3 1.9763(13) . ?
Ti O5 2.1499(12) . ?
Ti N1 2.2191(16) . ?
P O1 1.5369(14) . ?
P O2 1.5380(13) . ?
P O3 1.5394(13) 3 ?
P O4 1.5416(13) 4_565 ?
O3 P 1.5394(13) 3 ?
O4 P 1.5416(13) 4_566 ?
O5 Ti 1.7192(12) 2_545 ?
N1 C2 1.472(2) . ?
N1 H1 0.83(4) . ?
N1 H2 0.83(4) . ?
N2 C1 1.498(2) . ?
N2 H3 0.88(3) . ?
N2 H4 0.86(3) . ?
N2 H5 0.90(3) . ?
C1 C2 1.528(3) . ?
C1 H6 0.96(3) . ?
C1 H7 0.95(3) . ?
C2 H8 0.97(3) . ?
C2 H9 1.03(3) . ?
