#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006659.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_2006659
loop_
_publ_author_name
'Serpaggi, F.'
'Loiseau, T.'
'F\'erey, G.'
_publ_section_title
;
 A New Gallium Phosphate Templated by Tris(2-aminoethyl)amine:
 [Ga(HPO~4~)(PO~4~)(OH)].[(C~2~H~7~ N)~3~N].H~2~O
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1568
_journal_page_last               1570
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Ga (H P O4) (P O4) O H], C6 H21 N4, H2 O'
_chemical_formula_sum            'C6 H25 Ga N4 O10 P2'
_chemical_formula_weight         444.72
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.423(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4881(10)
_cell_length_b                   10.3231(11)
_cell_length_c                   16.3226(11)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32
_cell_measurement_theta_min      30
_cell_volume                     1598.7(3)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1988a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1988b)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1996)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990) option TREF 20'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Stoe Siemens AED-2 diffractometer'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2998
_diffrn_reflns_theta_max         29.95
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        5.2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.979
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type
'integration from crystal shape (Sheldrick, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       'prismatic platelet'
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.418
_exptl_crystal_size_mid          0.361
_exptl_crystal_size_min          0.068
_refine_diff_density_max         .863
_refine_diff_density_min         -.501
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.955
_refine_ls_goodness_of_fit_obs   1.056
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_restrained_S_obs      1.056
_refine_ls_R_factor_all          0.078
_refine_ls_R_factor_obs          0.042
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.133
_refine_ls_wR_factor_obs         0.120
_reflns_number_observed          1971
_reflns_number_total             2891
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    du1179.cif
_[local]_cod_data_source_block   I
_[local]_cod_chemical_formula_sum_orig 'C6 H25 Ga1 N4 O10 P2'
_cod_database_code               2006659
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_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ga1 0.0427(3) 0.0227(3) 0.0254(3) 0.0050(2) -0.0099(2) 0.0008(2)
P1 0.0262(5) 0.0192(6) 0.0228(6) 0.0016(4) -0.0026(4) -0.0012(4)
P2 0.0481(6) 0.0181(6) 0.0218(6) 0.0018(4) 0.0065(5) -0.0015(4)
O1 0.0278(14) 0.033(2) 0.038(2) -0.0031(12) -0.0011(13) 0.0029(14)
O2 0.034(2) 0.025(2) 0.033(2) 0.0032(12) -0.0029(12) -0.0016(14)
O3 0.052(2) 0.035(2) 0.032(2) 0.0142(15) 0.0077(14) 0.0037(15)
O4 0.042(2) 0.025(2) 0.022(2) -0.0027(12) 0.0029(12) -0.0028(12)
O5 0.044(2) 0.025(2) 0.047(2) 0.0108(14) -0.0099(15) -0.0080(15)
O6 0.048(2) 0.027(2) 0.026(2) -0.0074(13) -0.0082(13) -0.0048(13)
O7 0.090(3) 0.043(2) 0.027(2) 0.034(2) -0.004(2) -0.005(2)
O8 0.115(3) 0.038(2) 0.060(3) -0.037(2) 0.047(2) -0.023(2)
O9 0.106(4) 0.046(3) 0.117(4) 0.028(2) -0.092(3) -0.007(3)
Ow 0.080(4) 0.156(7) 0.292(12) -0.035(4) 0.014(6) -0.089(8)
N1 0.024(2) 0.024(2) 0.024(2) -0.0018(13) -0.0015(13) -0.0016(14)
N2 0.044(2) 0.020(2) 0.049(3) 0.003(2) -0.001(2) 0.003(2)
N3 0.038(2) 0.025(2) 0.026(2) -0.0090(15) -0.0043(15) 0.0026(15)
N4 0.036(2) 0.028(2) 0.021(2) -0.0042(15) -0.0041(14) 0.001(2)
C1 0.028(2) 0.035(2) 0.030(2) 0.005(2) 0.000(2) -0.005(2)
C2 0.026(2) 0.034(2) 0.033(2) -0.007(2) 0.002(2) 0.005(2)
C3 0.034(2) 0.030(2) 0.026(2) -0.003(2) 0.002(2) -0.005(2)
C4 0.043(2) 0.024(2) 0.039(3) -0.010(2) 0.000(2) 0.001(2)
C5 0.046(3) 0.027(2) 0.026(2) -0.001(2) -0.006(2) 0.001(2)
C6 0.029(2) 0.033(2) 0.028(2) -0.006(2) -0.010(2) -0.001(2)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Ga1 0.66631(5) 0.11477(4) 0.56708(3) 0.0303(2) Uani d . 1 Ga
P1 0.63790(10) 0.11211(10) 0.12335(7) 0.0227(3) Uani d . 1 P
P2 0.40784(12) -0.04470(11) 0.61348(7) 0.0293(3) Uani d . 1 P
O1 0.4793(3) 0.0990(3) 0.1334(2) 0.0329(7) Uani d . 1 O
O2 0.4849(3) -0.1722(3) 0.6176(2) 0.0307(7) Uani d . 1 O
O3 0.2973(3) -0.0264(3) 0.6788(2) 0.0400(8) Uani d . 1 O
O4 0.6686(3) 0.2110(3) 0.0535(2) 0.0297(7) Uani d . 1 O
O5 0.7116(3) -0.0131(3) 0.1090(2) 0.0386(8) Uani d . 1 O
O6 0.6997(3) 0.1806(3) 0.2022(2) 0.0337(7) Uani d . 1 O
O7 0.3364(4) -0.0285(4) 0.5289(2) 0.0534(10) Uani d . 1 O
O8 0.5117(5) 0.0708(4) 0.6237(2) 0.0708(14) Uani d . 1 O
O9 0.8100(5) 0.0600(4) 0.6266(3) 0.090(2) Uani d . 1 O
Ow 1.0331(7) -0.0755(8) 0.5989(6) 0.176(4) Uani d . 1 O
N1 0.1396(3) 0.1242(3) 0.1387(2) 0.0239(8) Uani d . 1 N
N2 0.3200(4) -0.1145(3) 0.1679(3) 0.0377(10) Uani d . 1 N
HN2A 0.3685(12) -0.1810(19) 0.1480(15) 0.057 Uiso calc R 1 H
HN2B 0.3125(4) -0.123(3) 0.2220(3) 0.057 Uiso calc R 1 H
HN2C 0.3647(13) -0.0409(14) 0.1564(17) 0.057 Uiso calc R 1 H
N3 0.3260(4) 0.2023(3) -0.0012(2) 0.0298(8) Uani d . 1 N
HN3A 0.3802(10) 0.2637(9) -0.0227(17) 0.045 Uiso calc R 1 H
HN3B 0.3640(13) 0.175(3) 0.0458(4) 0.045 Uiso calc R 1 H
HN3C 0.3193(5) 0.1361(19) -0.0359(15) 0.045 Uiso calc R 1 H
N4 0.3404(3) 0.2620(3) 0.2485(2) 0.0287(8) Uani d . 1 N
HN4A 0.3977(6) 0.249(3) 0.2912(6) 0.043 Uiso calc R 1 H
HN4B 0.3441(7) 0.3449(9) 0.2337(18) 0.043 Uiso calc R 1 H
HN4C 0.3671(12) 0.212(2) 0.2069(13) 0.043 Uiso calc R 1 H
C1 0.0970(4) 0.2247(4) 0.1973(3) 0.0310(10) Uani d . 1 C
HC1A 0.0014(4) 0.2078(4) 0.2150(3) 0.037 Uiso calc R 1 H
HC1B 0.0981(4) 0.3084(4) 0.1704(3) 0.037 Uiso calc R 1 H
C2 0.0866(4) -0.0046(4) 0.1634(3) 0.0310(10) Uani d . 1 C
HC2A' -0.0093(4) -0.0153(4) 0.1435(3) 0.037 Uiso calc R 1 H
HC2B' 0.0851(4) -0.0099(4) 0.2227(3) 0.037 Uiso calc R 1 H
C3 0.1942(4) 0.2286(4) 0.2717(3) 0.0298(9) Uani d . 1 C
HC3A' 0.1595(4) 0.2922(4) 0.3104(3) 0.036 Uiso calc R 1 H
HC3B' 0.1937(4) 0.1447(4) 0.2985(3) 0.036 Uiso calc R 1 H
C4 0.1771(5) -0.1122(4) 0.1302(3) 0.0357(11) Uani d . 1 C
HC4A' 0.1311(5) -0.1945(4) 0.1401(3) 0.043 Uiso calc R 1 H
HC4B' 0.1860(5) -0.1016(4) 0.0714(3) 0.043 Uiso calc R 1 H
C5 0.1842(5) 0.2554(4) 0.0143(3) 0.0329(10) Uani d . 1 C
HC5A 0.1922(5) 0.3312(4) 0.0492(3) 0.039 Uiso calc R 1 H
HC5B 0.1415(5) 0.2820(4) -0.0371(3) 0.039 Uiso calc R 1 H
C6 0.0912(4) 0.1562(5) 0.0552(3) 0.0302(10) Uani d . 1 C
HC6A -0.0043(4) 0.1894(5) 0.0575(3) 0.036 Uiso calc R 1 H
HC6B 0.0897(4) 0.0779(5) 0.0223(3) 0.036 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
Ga Ga .2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .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
_geom_angle_publ_flag
O9 Ga1 O8 . . 105.5(3) yes
O9 Ga1 O7 . 3_656 109.0(2) yes
O8 Ga1 O7 . 3_656 108.4(2) yes
O9 Ga1 O4 . 4_566 112.1(2) yes
O8 Ga1 O4 . 4_566 108.9(2) yes
O7 Ga1 O4 3_656 4_566 112.6(2) yes
O5 P1 O1 . . 114.0(2) yes
O5 P1 O4 . . 111.2(2) yes
O1 P1 O4 . . 109.1(2) yes
O5 P1 O6 . . 110.2(2) yes
O1 P1 O6 . . 108.3(2) yes
O4 P1 O6 . . 103.5(2) yes
O2 P2 O3 . . 114.6(2) yes
O2 P2 O7 . . 110.1(2) yes
O3 P2 O7 . . 108.4(2) yes
O2 P2 O8 . . 111.0(2) yes
O3 P2 O8 . . 105.7(2) yes
O7 P2 O8 . . 106.7(2) yes
P1 O4 Ga1 . 4_565 123.9(2) yes
P2 O7 Ga1 . 3_656 136.7(2) yes
P2 O8 Ga1 . . 131.0(2) yes
C1 N1 C6 . . 111.0(3) yes
C1 N1 C2 . . 111.1(3) yes
C6 N1 C2 . . 110.5(3) yes
N1 C1 C3 . . 111.8(3) yes
N1 C2 C4 . . 111.6(3) yes
N4 C3 C1 . . 111.5(3) yes
N2 C4 C2 . . 112.5(4) yes
N3 C5 C6 . . 111.1(4) yes
N1 C6 C5 . . 112.4(3) yes
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
Ga1 O9 . 1.761(4) yes
Ga1 O8 . 1.798(4) yes
Ga1 O7 3_656 1.802(3) yes
Ga1 O4 4_566 1.812(3) yes
P1 O5 . 1.489(3) yes
P1 O1 . 1.521(3) yes
P1 O4 . 1.559(3) yes
P1 O6 . 1.578(3) yes
P2 O2 . 1.506(3) yes
P2 O3 . 1.513(3) yes
P2 O7 . 1.543(4) yes
P2 O8 . 1.555(4) yes
O4 Ga1 4_565 1.812(3) ?
O7 Ga1 3_656 1.802(3) ?
N1 C1 . 1.469(5) yes
N1 C6 . 1.473(5) yes
N1 C2 . 1.479(5) yes
N2 C4 . 1.485(6) yes
N3 C5 . 1.476(6) yes
N4 C3 . 1.481(5) yes
C1 C3 . 1.520(6) yes
C2 C4 . 1.508(6) yes
C5 C6 . 1.510(6) ?
C6 C5 . 1.510(6) yes