#------------------------------------------------------------------------------
#$Date: 2020-03-27 12:18:32 +0200 (Fri, 27 Mar 2020) $
#$Revision: 249787 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/90/2009050.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2009050
loop_
_publ_author_name
'Sugiyama, Kazumasa'
'Hiraga, Kenji'
'Yu,  Jihong'
'Zheng, Shan'
'Qiu, Shilun'
'Xu, Ruren'
'Terasaki, Osamu'
_publ_section_title
;
 A one-dimensionally extended chain aluminophosphate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1615
_journal_page_last               1617
_journal_paper_doi               10.1107/S0108270199000360
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '(C2 H10 N2)(C3 H12 N2 )2 [Al2 P4 O16 ]'
_chemical_formula_moiety
'(C2 H10 N2 2+)(C3 H12 N2 2+)2 [Al2 P4 O16 6-]'
_chemical_formula_sum            'C8 H34 Al2 N6 O16 P4'
_chemical_formula_weight         648.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                115.764(8)
_cell_angle_beta                 99.704(11)
_cell_angle_gamma                98.247(11)
_cell_formula_units_Z            1
_cell_length_a                   8.9499(12)
_cell_length_b                   9.2513(9)
_cell_length_c                   8.6473(11)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      16.65
_cell_measurement_theta_min      15.15
_cell_volume                     616.35(15)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
 1988)
;
_computing_molecular_graphics    'ATOMS (Dowty, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC-7R'
_diffrn_measurement_method       ' ω-2θ scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3761
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.462
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_type   '\y-scan (North et al., 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             338
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.353
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0412P)²+0.2842P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                2695
_reflns_number_total             3599
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            oh1114.cif
_cod_data_source_block           97040
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0412P)^2^+0.2842P] 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^)+(0.0412P)^2^+0.2842P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

2019-11-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C4 H17 Al N3 O8 P2'
_cod_original_formula_weight         324.13
_cod_original_formula_units_Z            2
_cod_original_cell_volume        616.40(10)
_cod_database_code               2009050
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
P1 .41784(6) .26023(7) .75432(8) .01498(13) Uani d . 1 . . P
P2 .97718(7) .33548(8) .10561(8) .01596(13) Uani d . 1 . . P
Al1 .74612(7) .50134(8) .97468(9) .01360(14) Uani d . 1 . . Al
O1 .85136(19) .5672(2) .8550(2) .0215(4) Uani d . 1 . . O
O2 .6632(2) .6575(2) .0964(2) .0241(4) Uani d . 1 . . O
O3 .87147(19) .4569(2) .1150(2) .0218(4) Uani d . 1 . . O
O4 .40346(19) .6710(2) .1686(2) .0263(4) Uani d . 1 . . O
O5 .6370(2) .7031(2) .3966(3) .0285(4) Uani d . 1 . . O
O6 .6185(2) .9231(2) .3022(3) .0260(4) Uani d . 1 . . O
O7 .0713(2) .8149(2) .0746(3) .0324(5) Uani d . 1 . . O
O8 .9709(2) .3007(2) .2610(2) .0241(4) Uani d . 1 . . O
N11 .7660(2) .4691(3) .4428(3) .0257(5) Uani d . 1 . . N
H111 .8274 .4213 .3752 .053(3) Uiso calc R 1 . . H
H112 .8199 .5217 .5565 .053(3) Uiso calc R 1 . . H
H113 .7322 .5412 .4121 .053(3) Uiso calc R 1 . . H
C12 .6301(3) .3405(4) .4173(4) .0297(6) Uani d . 1 . . C
H121 .5613 .3925 .4880 .053(3) Uiso calc R 1 . . H
H122 .6662 .2651 .4567 .053(3) Uiso calc R 1 . . H
C13 .5419(4) .2456(4) .2231(4) .0385(7) Uani d . 1 . . C
H131 .5995 .1676 .1604 .053(3) Uiso calc R 1 . . H
H132 .5402 .3230 .1755 .053(3) Uiso calc R 1 . . H
C14 .3747(4) .1509(4) .1828(4) .0383(7) Uani d . 1 . . C
H141 .3106 .2292 .2223 .053(3) Uiso calc R 1 . . H
H142 .3345 .0827 .0552 .053(3) Uiso calc R 1 . . H
N15 .3612(3) .0441(2) .2696(2) .0303(5) Uani d . 1 . . N
H151 .4421 -.0020 .2659 .053(3) Uiso calc R 1 . . H
H152 .2728 -.0347 .2127 .053(3) Uiso calc R 1 . . H
H153 .3607 .1051 .3823 .053(3) Uiso calc R 1 . . H
N21 .0798(2) .9778(2) .7025(2) .0220(4) Uani d R 1 . . N
H211 .1722 1.0475 .7340 .053(3) Uiso calc R 1 . . H
H212 .0936 .8894 .7145 .053(3) Uiso calc R 1 . . H
H213 .0206 1.0280 .7719 .053(3) Uiso calc R 1 . . H
C22 .0019(3) .9254(3) .5152(4) .0255(5) Uani d . 1 . . C
H221 -.1041 .8614 .4855 .053(3) Uiso calc R 1 . . H
H222 .0575 .8555 .4380 .053(3) Uiso calc R 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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'
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O5 P1 O6 2_666 2_666 112.79(12)
O5 P1 O4 2_666 2_666 110.14(11)
O6 P1 O4 2_666 2_666 107.73(10)
O5 P1 O2 2_666 2_666 109.88(10)
O6 P1 O2 2_666 2_666 107.45(11)
O4 P1 O2 2_666 2_666 108.73(10)
O7 P2 O8 2_665 . 115.22(12)
O7 P2 O3 2_665 . 110.78(11)
O8 P2 O3 . . 106.34(10)
O7 P2 O1 2_665 2_766 111.02(11)
O8 P2 O1 . 2_766 106.18(10)
O3 P2 O1 . 2_766 106.83(10)
O4 Al1 O2 2_666 1_556 107.85(9)
O4 Al1 O3 2_666 1_556 110.43(10)
O2 Al1 O3 1_556 1_556 110.43(9)
O4 Al1 O1 2_666 . 110.28(9)
O2 Al1 O1 1_556 . 108.61(9)
O3 Al1 O1 1_556 . 109.22(9)
P2 O1 Al1 2_766 . 134.58(11)
P1 O2 Al1 2_666 1_554 151.81(13)
P2 O3 Al1 . 1_554 139.90(12)
P1 O4 Al1 2_666 2_666 145.74(12)
C12 N11 H111 . . 109.5
C12 N11 H112 . . 109.5
H111 N11 H112 . . 109.5
C12 N11 H113 . . 109.5
H111 N11 H113 . . 109.5
H112 N11 H113 . . 109.5
N11 C12 C13 . . 109.8(2)
N11 C12 H121 . . 109.7
C13 C12 H121 . . 109.7
N11 C12 H122 . . 109.7
C13 C12 H122 . . 109.7
H121 C12 H122 . . 108.2
C12 C13 C14 . . 116.0(3)
C12 C13 H131 . . 108.3
C14 C13 H131 . . 108.3
C12 C13 H132 . . 108.3
C14 C13 H132 . . 108.3
H131 C13 H132 . . 107.4
N15 C14 C13 . . 112.9(2)
N15 C14 H141 . . 109.0
C13 C14 H141 . . 109.0
N15 C14 H142 . . 109.0
C13 C14 H142 . . 109.0
H141 C14 H142 . . 107.8
C14 N15 H151 . . 109.5
C14 N15 H152 . . 109.5
H151 N15 H152 . . 109.5
C14 N15 H153 . . 109.5
H151 N15 H153 . . 109.5
H152 N15 H153 . . 109.5
C22 N21 H211 . . 109.5
C22 N21 H212 . . 109.5
H211 N21 H212 . . 109.5
C22 N21 H213 . . 109.5
H211 N21 H213 . . 109.5
H212 N21 H213 . . 109.5
N21 C22 C22 . 2_576 110.7(3)
N21 C22 H221 . . 109.5
C22 C22 H221 2_576 . 109.5
N21 C22 H222 . . 109.5
C22 C22 H222 2_576 . 109.5
H221 C22 H222 . . 108.1
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
P1 O5 2_666 1.509(2) yes
P1 O6 2_666 1.513(2) yes
P1 O4 2_666 1.545(2) yes
P1 O2 2_666 1.546(2) yes
P2 O7 2_665 1.506(2) yes
P2 O8 . 1.519(2) yes
P2 O3 . 1.554(2) yes
P2 O1 2_766 1.563(2) yes
Al1 O4 2_666 1.726(2) yes
Al1 O2 1_556 1.731(2) yes
Al1 O3 1_556 1.734(2) yes
Al1 O1 . 1.745(2) yes
O1 P2 2_766 1.563(2) ?
O2 P1 2_666 1.546(2) ?
O2 Al1 1_554 1.731(2) ?
O3 Al1 1_554 1.733(2) ?
O4 P1 2_666 1.545(2) ?
O4 Al1 2_666 1.726(2) ?
O5 P1 2_666 1.509(2) ?
O6 P1 2_666 1.513(2) ?
O7 P2 2_665 1.506(2) ?
N11 C12 . 1.486(3) yes
N11 H111 . .8900 ?
N11 H112 . .8900 ?
N11 H113 . .8900 ?
C12 C13 . 1.512(4) yes
C12 H121 . .9700 ?
C12 H122 . .9700 ?
C13 C14 . 1.520(4) yes
C13 H131 . .9700 ?
C13 H132 . .9700 ?
C14 N15 . 1.481(3) yes
C14 H141 . .9700 ?
C14 H142 . .9700 ?
N15 H151 . .8900 ?
N15 H152 . .8900 ?
N15 H153 . .8900 ?
N21 C22 . 1.478(3) yes
N21 H211 . .8900 ?
N21 H212 . .8900 ?
N21 H213 . .8900 ?
C22 C22 2_576 1.516(5) yes
C22 H221 . .9700 ?
C22 H222 . .9700 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N11 H111 O8 . 0.89 1.937 2.815(3) 168.6 yes
N11 H111 O3 . 0.89 2.500 3.098(3) 125.3 ?
N11 H112 O8 2_766 0.89 2.136 2.903(3) 143.9 yes
N11 H112 O1 . 0.89 2.386 3.190(3) 150.4 ?
N11 H113 O5 . 0.89 1.868 2.738(3) 165.0 yes
N15 H151 O6 1_545 0.89 1.846 2.726(3) 169.7 yes
N15 H152 O7 1_545 0.89 1.929 2.812(3) 171.5 yes
N15 H153 O5 2_666 0.89 1.958 2.812(3) 160.4 yes
N21 H211 O6 2_676 0.89 1.951 2.737(3) 146.4 yes
N21 H212 O8 2_666 0.89 1.884 2.714(2) 154.4 yes
N21 H213 O7 2_576 0.89 1.894 2.763(3) 164.9 yes
