#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/20/40/7204074.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_7204074
loop_
_publ_author_name
'Wragg, David S.'
'Slawin, Alexandra M. Z.'
'Morris, Russell E.'
_publ_section_title
;
 The synthesis of gallium phosphate frameworks with and without
 fluoride ions present: attempts to direct the synthesis of double
 four-ring containing materials
;
_journal_issue                   7
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              1850
_journal_paper_doi               10.1039/b100471i
_journal_volume                  11
_journal_year                    2001
_chemical_formula_sum            'C10 H14 F2 Ga6 N2 O25 P6'
_chemical_formula_weight         1204.36
_space_group_IT_number           2
_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
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta3
_audit_creation_date             1999-09-14T10:05:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                94.36(6)
_cell_angle_beta                 90.64(5)
_cell_angle_gamma                103.67(5)
_cell_formula_units_Z            1
_cell_length_a                   9.265(5)
_cell_length_b                   9.397(8)
_cell_length_c                   9.238(5)
_cell_measurement_temperature    293(2)
_cell_volume                     778.9(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2730
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    5.538
_exptl_crystal_density_diffrn    2.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             582
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.136
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                2518
_reflns_number_total             2730
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100471i.txt
_cod_data_source_block           '[pyr,F]-GaPO-2'
_cod_database_code               7204074
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_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
Ga1 Ga 0.13908(4) 0.08599(4) 0.43565(4) 0.01163(12) Uani 1 1 d . . .
Ga2 Ga 0.60890(4) 0.34138(4) 0.39230(4) 0.01249(13) Uani 1 1 d . . .
Ga3 Ga 0.62500(4) -0.07859(4) 0.15717(4) 0.01277(13) Uani 1 1 d . . .
P4 P 0.37722(10) 0.09021(10) 0.18526(10) 0.0118(2) Uani 1 1 d . . .
P5 P 0.37956(10) 0.32951(10) 0.62664(10) 0.0116(2) Uani 1 1 d . . .
P6 P 0.83224(10) 0.14986(10) 0.35659(10) 0.0131(2) Uani 1 1 d . . .
F1 F -0.0201(2) -0.0906(2) 0.3875(2) 0.0157(4) Uani 1 1 d . . .
O1 O 0.4394(3) -0.0469(3) 0.1776(4) 0.0296(7) Uani 1 1 d . . .
O2 O 0.2712(3) 0.2667(3) 0.5023(3) 0.0180(6) Uani 1 1 d . . .
O3 O 0.5396(3) 0.3462(3) 0.5747(3) 0.0225(6) Uani 1 1 d . . .
O4 O 0.7686(3) 0.0884(3) 0.2025(3) 0.0196(6) Uani 1 1 d . . .
O5 O 0.7891(3) 0.2975(3) 0.3915(3) 0.0189(6) Uani 1 1 d . . .
O6 O 0.2367(3) -0.0403(3) 0.5361(3) 0.0179(6) Uani 1 1 d . . .
O7 O 0.2276(3) 0.0597(3) 0.2551(3) 0.0190(6) Uani 1 1 d . . .
O8 O 0.6427(3) -0.2405(3) 0.2413(3) 0.0194(6) Uani 1 1 d . . .
O9 O 0.0016(3) 0.1882(3) 0.3533(3) 0.0163(6) Uani 1 1 d . . .
O10 O 0.4877(3) 0.2185(4) 0.2622(4) 0.0350(8) Uani 1 1 d . . .
O11 O 0.3589(4) 0.4812(3) 0.6819(3) 0.0238(6) Uani 1 1 d . . .
O12 O 0.3543(4) 0.1329(4) 0.0320(3) 0.0320(7) Uani 1 1 d . . .
C1 C 0.8795(9) 0.5342(14) 0.7574(11) 0.089(3) Uani 1 1 d . . .
H1 H 0.9137 0.6047 0.6924 0.107 Uiso 1 1 calc R . .
C2 C 0.9200(11) 0.4161(17) 0.7428(10) 0.106(4) Uani 1 1 d . . .
H2 H 0.9758 0.3988 0.6631 0.127 Uiso 1 1 calc R . .
C3 C 0.8862(11) 0.3151(9) 0.8369(16) 0.097(3) Uani 1 1 d . . .
H3 H 0.9195 0.2291 0.8242 0.116 Uiso 1 1 calc R . .
N1 N 0.7559(9) 0.4692(12) 0.9607(9) 0.118(3) Uani 1 1 d . . .
H1A H 0.7028 0.4911 1.0309 0.141 Uiso 1 1 calc R . .
C5 C 0.8011(11) 0.5605(10) 0.8485(14) 0.098(3) Uani 1 1 d . . .
H5 H 0.7671 0.6459 0.8464 0.117 Uiso 1 1 calc R . .
C4 C 0.8060(13) 0.3366(10) 0.9475(11) 0.100(4) Uani 1 1 d . . .
H4 H 0.7821 0.2677 1.0159 0.119 Uiso 1 1 calc R . .
O21 O -0.0181(12) -0.0896(12) 0.0258(11) 0.079(3) Uani 0.5 1 d P . .
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'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
O7 Ga1 O2 97.29(13) . . ?
O7 Ga1 O6 95.55(13) . . ?
O2 Ga1 O6 96.88(13) . . ?
O7 Ga1 O9 92.84(12) . . ?
O2 Ga1 O9 91.40(13) . . ?
O6 Ga1 O9 167.36(11) . . ?
O7 Ga1 F1 90.99(12) . . ?
O2 Ga1 F1 170.88(10) . . ?
O6 Ga1 F1 86.06(12) . . ?
O9 Ga1 F1 84.35(12) . . ?
O7 Ga1 F1 171.35(10) . 2_556 ?
O2 Ga1 F1 91.05(12) . 2_556 ?
O6 Ga1 F1 85.70(11) . 2_556 ?
O9 Ga1 F1 84.62(11) . 2_556 ?
F1 Ga1 F1 80.54(11) . 2_556 ?
O7 Ga1 Ga1 131.54(10) . 2_556 ?
O2 Ga1 Ga1 130.92(9) . 2_556 ?
O6 Ga1 Ga1 84.59(10) . 2_556 ?
O9 Ga1 Ga1 82.76(9) . 2_556 ?
F1 Ga1 Ga1 40.57(7) . 2_556 ?
F1 Ga1 Ga1 39.96(7) 2_556 2_556 ?
O10 Ga2 O5 109.13(14) . . ?
O10 Ga2 O3 114.80(15) . . ?
O5 Ga2 O3 110.74(13) . . ?
O10 Ga2 O11 104.78(17) . 2_666 ?
O5 Ga2 O11 104.47(14) . 2_666 ?
O3 Ga2 O11 112.27(14) . 2_666 ?
O8 Ga3 O12 101.19(15) . 2_655 ?
O8 Ga3 O4 116.91(14) . . ?
O12 Ga3 O4 106.57(15) 2_655 . ?
O8 Ga3 O1 111.45(14) . . ?
O12 Ga3 O1 108.04(16) 2_655 . ?
O4 Ga3 O1 111.68(14) . . ?
O7 P4 O10 112.76(17) . . ?
O7 P4 O12 107.36(18) . . ?
O10 P4 O12 106.4(2) . . ?
O7 P4 O1 110.32(17) . . ?
O10 P4 O1 110.15(19) . . ?
O12 P4 O1 109.70(19) . . ?
O2 P5 O8 114.12(17) . 2_656 ?
O2 P5 O11 109.55(17) . . ?
O8 P5 O11 104.80(16) 2_656 . ?
O2 P5 O3 109.68(16) . . ?
O8 P5 O3 109.67(17) 2_656 . ?
O11 P5 O3 108.82(18) . . ?
O6 P6 O9 115.96(16) 2_656 1_655 ?
O6 P6 O5 110.27(17) 2_656 . ?
O9 P6 O5 105.48(16) 1_655 . ?
O6 P6 O4 108.37(16) 2_656 . ?
O9 P6 O4 108.81(16) 1_655 . ?
O5 P6 O4 107.65(17) . . ?
Ga1 F1 Ga1 99.46(11) . 2_556 ?
P4 O1 Ga3 133.99(19) . . ?
P5 O2 Ga1 139.28(18) . . ?
P5 O3 Ga2 130.05(18) . . ?
P6 O4 Ga3 126.44(18) . . ?
P6 O5 Ga2 130.66(17) . . ?
P6 O6 Ga1 126.85(17) 2_656 . ?
P4 O7 Ga1 141.12(18) . . ?
P5 O8 Ga3 148.60(18) 2_656 . ?
P6 O9 Ga1 128.27(16) 1_455 . ?
P4 O10 Ga2 165.0(3) . . ?
P5 O11 Ga2 134.64(18) . 2_666 ?
P4 O12 Ga3 142.2(2) . 2_655 ?
C5 C1 C2 123.4(9) . . ?
C1 C2 C3 122.2(9) . . ?
C4 C3 C2 119.5(9) . . ?
C5 N1 C4 113.7(8) . . ?
C1 C5 N1 122.9(9) . . ?
C3 C4 N1 117.9(8) . . ?
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
Ga1 O7 1.892(3) . ?
Ga1 O2 1.898(3) . ?
Ga1 O6 1.935(3) . ?
Ga1 O9 1.947(3) . ?
Ga1 F1 1.960(3) . ?
Ga1 F1 1.985(2) 2_556 ?
Ga1 Ga1 3.010(2) 2_556 ?
Ga2 O10 1.785(3) . ?
Ga2 O5 1.811(3) . ?
Ga2 O3 1.811(3) . ?
Ga2 O11 1.811(3) 2_666 ?
Ga3 O8 1.800(3) . ?
Ga3 O12 1.808(3) 2_655 ?
Ga3 O4 1.819(3) . ?
Ga3 O1 1.823(3) . ?
P4 O7 1.510(3) . ?
P4 O10 1.509(3) . ?
P4 O12 1.527(3) . ?
P4 O1 1.528(3) . ?
P5 O2 1.505(3) . ?
P5 O8 1.520(3) 2_656 ?
P5 O11 1.533(3) . ?
P5 O3 1.540(3) . ?
P6 O6 1.519(3) 2_656 ?
P6 O9 1.526(3) 1_655 ?
P6 O5 1.545(3) . ?
P6 O4 1.550(3) . ?
F1 Ga1 1.985(2) 2_556 ?
O6 P6 1.519(3) 2_656 ?
O8 P5 1.520(3) 2_656 ?
O9 P6 1.526(3) 1_455 ?
O11 Ga2 1.811(3) 2_666 ?
O12 Ga3 1.808(3) 2_655 ?
C1 C5 1.168(13) . ?
C1 C2 1.252(14) . ?
C2 C3 1.321(15) . ?
C3 C4 1.302(14) . ?
N1 C5 1.400(13) . ?
N1 C4 1.427(13) . ?
O21 O21 1.74(2) 2 ?
