#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/08/4500812.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_4500812
loop_
_publ_author_name
'Olshansky, Jacob H.'
'Blau, Samuel M.'
'Zeller, Matthias'
'Schrier, Joshua'
'Norquist, Alexander J.'
_publ_section_title
;
 Understanding an Order--Disorder Phase Transition in Ionothermally
 Synthesized Gallium Phosphates
;
_journal_issue                   7
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3065
_journal_paper_doi               10.1021/cg200332y
_journal_volume                  11
_journal_year                    2011
_chemical_formula_moiety         'C5 H15 Ga1 N2 O8 P2'
_chemical_formula_sum            'C5 H15 Ga N2 O8 P2'
_chemical_formula_weight         362.85
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                92.195(3)
_cell_angle_beta                 95.709(3)
_cell_angle_gamma                98.509(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4510(19)
_cell_length_b                   8.777(2)
_cell_length_c                   8.928(2)
_cell_measurement_reflns_used    7745
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.3472
_cell_measurement_theta_min      3
_cell_volume                     650.7(3)
_computing_cell_refinement       APEX2
_computing_data_collection       APEX2
_computing_data_reduction        APEX2
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device       'Bruker AXS Smart Apex CCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7744
_diffrn_reflns_theta_full        25.787
_diffrn_reflns_theta_max         31.448
_diffrn_reflns_theta_min         2.296
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.393
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   APEX2
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.00
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8254
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3423
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.0002670
_refine_ls_shift/su_mean         0.0644745
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 39.4 58.2 32.7 9.32 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0749
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0722
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                3555
_reflns_number_total             3904
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   0.57
_oxford_diffrn_Wilson_scale      1.34
_oxford_refine_ls_r_factor_ref   0.0262
_oxford_refine_ls_scale          0.8021(17)
_oxford_reflns_number_all        3893
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            cg200332y_si_002.cif
_cod_data_source_block           '[C~5~H~14~N~2~][Ga(HPO~4~)(PO~4~)]_Cmp-1b'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C5 H15 Ga1 N2 O8 P2'
_cod_database_code               4500812
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
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_occupancy
_atom_site_adp_type
Ga1 Ga 0.01133(2) 0.48307(2) 0.252214(19) 0.0081 1.0000 Uani
P1 P -0.00268(5) 0.73261(5) 0.01911(5) 0.0087 1.0000 Uani
P2 P 0.23640(5) 0.56364(5) 0.53101(5) 0.0092 1.0000 Uani
O1 O 0.08620(15) 0.63970(14) 0.13622(14) 0.0124 1.0000 Uani
O2 O -0.05230(15) 0.30306(14) 0.13783(14) 0.0121 1.0000 Uani
O3 O 0.18969(14) 0.46255(14) 0.38046(13) 0.0109 1.0000 Uani
O4 O -0.16181(15) 0.53130(15) 0.34150(14) 0.0121 1.0000 Uani
O5 O 0.06674(17) 0.90295(14) 0.06385(15) 0.0143 1.0000 Uani
O6 O -0.18179(15) 0.69697(17) 0.01836(15) 0.0162 1.0000 Uani
O7 O 0.42067(15) 0.57955(16) 0.56567(15) 0.0146 1.0000 Uani
O8 O 0.17596(17) 0.71549(15) 0.52354(15) 0.0162 1.0000 Uani
N1 N 0.45470(19) 0.4290(2) 0.13446(18) 0.0187 1.0000 Uani
N2 N 0.0601(3) 0.9349(2) 0.3725(2) 0.0265 1.0000 Uani
C1 C 0.5640(2) 0.3601(3) 0.0382(2) 0.0199 1.0000 Uani
C2 C 0.4724(2) 0.5996(3) 0.1244(2) 0.0189 1.0000 Uani
C3 C 0.5449(6) 0.1880(6) 0.0552(6) 0.0287 0.5000 Uani
C4 C 0.1485(3) 1.0786(3) 0.4517(3) 0.0274 1.0000 Uani
C5 C -0.1172(3) 0.9213(3) 0.3840(3) 0.0284 1.0000 Uani
C6 C 0.3144(7) 1.0828(6) 0.4375(8) 0.0385 0.5000 Uani
H1 H 0.0000 1.0000 0.0000 0.0500 1.0000 Uiso
H2 H 0.5000 0.5000 0.5000 0.0500 1.0000 Uiso
H3 H 0.4801 0.4059 0.2361 0.0226 1.0000 Uiso
H4 H 0.3466 0.3857 0.1014 0.0226 1.0000 Uiso
H5 H 0.6742 0.4029 0.0727 0.0244 1.0000 Uiso
H6 H 0.5491 0.2512 0.0457 0.0244 0.5000 Uiso
H7 H 0.5814 0.6440 0.1621 0.0223 1.0000 Uiso
H8 H 0.3975 0.6377 0.1850 0.0230 1.0000 Uiso
H9 H 0.5690 0.1682 0.1580 0.0430 0.5000 Uiso
H10 H 0.6161 0.1445 -0.0047 0.0431 0.5000 Uiso
H11 H 0.4362 0.1440 0.0210 0.0431 0.5000 Uiso
H12 H 0.0779 0.9345 0.2692 0.0336 1.0000 Uiso
H13 H 0.0986 0.8492 0.4172 0.0336 1.0000 Uiso
H14 H 0.1090 1.1653 0.4033 0.0352 1.0000 Uiso
H15 H 0.2603 1.0840 0.4441 0.0349 0.5000 Uiso
H16 H -0.1713 0.8260 0.3330 0.0348 1.0000 Uiso
H17 H -0.1476 1.0133 0.3405 0.0342 1.0000 Uiso
H18 H 0.3311 1.0797 0.3340 0.0439 0.5000 Uiso
H19 H 0.3490 0.9951 0.4828 0.0439 0.5000 Uiso
H20 H 0.3737 1.1740 0.4870 0.0439 0.5000 Uiso
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Ga 0.2307 1.6083 15.2354 3.0669 6.7006 0.2412 4.3591 10.7805 2.9623 61.4135
1.7189 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 . Ga1 O2 . 110.98(6) yes
O1 . Ga1 O3 . 102.98(6) yes
O2 . Ga1 O3 . 108.78(6) yes
O1 . Ga1 O4 . 109.88(6) yes
O2 . Ga1 O4 . 108.22(6) yes
O3 . Ga1 O4 . 115.94(6) yes
O2 2_565 P1 O1 . 107.97(7) yes
O2 2_565 P1 O5 . 106.51(7) yes
O1 . P1 O5 . 104.34(7) yes
O2 2_565 P1 O6 . 111.98(8) yes
O1 . P1 O6 . 111.85(8) yes
O5 . P1 O6 . 113.69(8) yes
O4 2_566 P2 O3 . 107.03(7) yes
O4 2_566 P2 O7 . 106.72(8) yes
O3 . P2 O7 . 106.96(7) yes
O4 2_566 P2 O8 . 110.22(8) yes
O3 . P2 O8 . 112.18(7) yes
O7 . P2 O8 . 113.37(8) yes
Ga1 . O1 P1 . 131.46(8) yes
Ga1 . O2 P1 2_565 125.10(8) yes
Ga1 . O3 P2 . 121.74(7) yes
Ga1 . O4 P2 2_566 123.01(8) yes
P1 . O5 H1 . 116.5 no
P2 . O7 H2 . 122.2 no
C1 . N1 C2 . 111.38(16) yes
C1 . N1 H3 . 109.0 no
C2 . N1 H3 . 109.0 no
C1 . N1 H4 . 108.9 no
C2 . N1 H4 . 108.8 no
H3 . N1 H4 . 109.7 no
C4 . N2 C5 . 111.40(18) yes
C4 . N2 H12 . 109.5 no
C5 . N2 H12 . 108.9 no
C4 . N2 H13 . 108.8 no
C5 . N2 H13 . 108.7 no
H12 . N2 H13 . 109.5 no
C2 2_665 C1 N1 . 109.51(15) yes
C2 2_665 C1 C3 . 112.2(3) yes
N1 . C1 C3 . 109.4(2) yes
C2 2_665 C1 H5 . 108.8 no
N1 . C1 H5 . 109.0 no
C3 . C1 H5 . 107.8 no
C2 2_665 C1 H6 . 110.4 no
N1 . C1 H6 . 109.5 no
C3 . C1 H6 . 2.1 no
H5 . C1 H6 . 109.6 no
C1 2_665 C2 N1 . 110.05(16) yes
C1 2_665 C2 H7 . 110.1 no
N1 . C2 H7 . 108.7 no
C1 2_665 C2 H8 . 109.5 no
N1 . C2 H8 . 108.2 no
H7 . C2 H8 . 110.3 no
C1 . C3 H6 . 3.6 no
C1 . C3 H9 . 109.4 no
H6 . C3 H9 . 112.6 no
C1 . C3 H10 . 109.4 no
H6 . C3 H10 . 109.2 no
H9 . C3 H10 . 109.9 no
C1 . C3 H11 . 108.7 no
H6 . C3 H11 . 105.7 no
H9 . C3 H11 . 110.0 no
H10 . C3 H11 . 109.3 no
C5 2_576 C4 N2 . 108.92(19) yes
C5 2_576 C4 C6 . 110.9(3) yes
N2 . C4 C6 . 108.2(3) yes
C5 2_576 C4 H14 . 110.6 no
N2 . C4 H14 . 107.7 no
C6 . C4 H14 . 110.4 no
C5 2_576 C4 H15 . 109.9 no
N2 . C4 H15 . 109.9 no
C6 . C4 H15 . 1.7 no
H14 . C4 H15 . 109.8 no
C4 2_576 C5 N2 . 109.81(19) yes
C4 2_576 C5 H16 . 109.1 no
N2 . C5 H16 . 109.5 no
C4 2_576 C5 H17 . 109.4 no
N2 . C5 H17 . 104.5 no
H16 . C5 H17 . 114.4 no
C4 . C6 H18 . 109.6 no
C4 . C6 H19 . 108.7 no
H18 . C6 H19 . 109.3 no
C4 . C6 H20 . 109.9 no
H18 . C6 H20 . 109.9 no
H19 . C6 H20 . 109.5 no
O5 2_575 H1 O5 . 180.0 no
O7 . H2 O7 2_666 180.0 no
C1 . H6 C3 . 174.2 no
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 O1 . 1.8288(13) yes
Ga1 O2 . 1.8287(13) yes
Ga1 O3 . 1.8353(12) yes
Ga1 O4 . 1.8290(13) yes
P1 O2 2_565 1.5544(13) yes
P1 O1 . 1.5532(13) yes
P1 O5 . 1.5449(13) yes
P1 O6 . 1.4990(14) yes
P2 O4 2_566 1.5644(13) yes
P2 O3 . 1.5650(13) yes
P2 O7 . 1.5416(14) yes
P2 O8 . 1.4977(14) yes
O5 H1 . 1.218 no
O7 H2 . 1.211 no
N1 C1 . 1.497(3) yes
N1 C2 . 1.490(3) yes
N1 H3 . 0.948 no
N1 H4 . 0.949 no
N2 C4 . 1.482(3) yes
N2 C5 . 1.499(4) yes
N2 H12 . 0.950 no
N2 H13 . 0.950 no
C1 C2 2_665 1.520(3) yes
C1 C3 . 1.510(5) yes
C1 H5 . 0.967 no
C1 H6 . 0.951 no
C2 H7 . 0.967 no
C2 H8 . 0.960 no
C3 H6 . 0.561 no
C3 H9 . 0.948 no
C3 H10 . 0.954 no
C3 H11 . 0.957 no
C4 C5 2_576 1.517(3) yes
C4 C6 . 1.415(6) yes
C4 H14 . 0.974 no
C4 H15 . 0.948 no
C5 H16 . 0.966 no
C5 H17 . 0.967 no
C6 H18 . 0.948 no
C6 H19 . 0.953 no
C6 H20 . 0.947 no
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_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
N1 H3 O7 2_666 161 0.95 1.87 2.786(5) yes
N1 H4 O6 2_565 159 0.95 1.72 2.628(5) yes
C2 H7 O6 1_655 128 0.97 2.48 3.168(5) yes
N2 H12 O5 . 166 0.95 1.83 2.767(5) yes
N2 H13 O8 . 170 0.95 1.70 2.642(5) yes
