#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/15/4111519.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_4111519
loop_
_publ_author_name
'Elisabeth Rather'
'Jason T. Gatlin'
'Paul G. Nixon'
'Takuji Tsukamoto'
'Victor Kravtsov'
'Darren W. Johnson'
_publ_section_title
;
 A Simple Organic Reaction Mediates the Crystallization of the Inorganic
 Nanocluster [Ga13(μ3-OH)6(μ2-OH)18(H2O)24](NO3)15
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3242
_journal_page_last               3243
_journal_paper_doi               10.1021/ja043520t
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'Ga13 H72 N15 O99'
_chemical_formula_weight         2773.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   20.214(3)
_cell_length_b                   20.214(3)
_cell_length_c                   18.353(4)
_cell_measurement_temperature    293(2)
_cell_volume                     6494(2)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12648
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    4.128
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.127
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             4116
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2831
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0716P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                2500
_reflns_number_total             2831
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja043520tsi20041104_114353.cif
_cod_data_source_block           jtg6hex
_cod_original_cell_volume        6494.7(19)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'H72 Ga13 N15 O99'
_cod_database_code               4111519
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 1.0000 1.0000 0.0000 0.0196(2) Uani 1 6 d S . .
Ga2 Ga 0.837137(19) 0.980265(18) -0.004021(17) 0.01921(13) Uani 1 1 d . . .
Ga3 Ga 0.697660(19) 0.821112(19) 0.09437(2) 0.02311(14) Uani 1 1 d . . .
O1 O 0.94201(11) 1.03770(11) -0.05420(13) 0.0206(5) Uani 1 1 d . . .
H1O H 0.9396 1.0376 -0.0992 0.025 Uiso 1 1 d R . .
O2 O 0.81260(13) 0.88619(12) -0.05055(12) 0.0220(5) Uani 1 1 d . . .
H2O H 0.8112 0.8833 -0.1001 0.026 Uiso 1 1 d R . .
O3 O 0.75336(12) 0.92485(12) 0.06121(12) 0.0236(5) Uani 1 1 d . . .
H3O H 0.7493 0.9539 0.0917 0.028 Uiso 1 1 d R . .
O4 O 0.79718(13) 1.02078(13) -0.07527(13) 0.0252(5) Uani 1 1 d . . .
H4O H 0.7547 0.9849 -0.0868 0.030 Uiso 1 1 d R . .
O5 O 0.73030(15) 0.85021(15) 0.19711(14) 0.0366(6) Uani 1 1 d . . .
H51W H 0.7705 0.8657 0.2083 0.044 Uiso 1 1 d R . .
H52W H 0.7124 0.8714 0.2221 0.044 Uiso 1 1 d R . .
O6 O 0.61213(14) 0.84161(15) 0.11670(16) 0.0383(6) Uani 1 1 d . . .
H61W H 0.5822 0.8181 0.1506 0.046 Uiso 1 1 d R . .
H62W H 0.6032 0.8682 0.0867 0.046 Uiso 1 1 d R . .
O7 O 0.62994(14) 0.71683(14) 0.13696(15) 0.0361(6) Uani 1 1 d . . .
H72W H 0.6164 0.6791 0.1078 0.043 Uiso 1 1 d R . .
H71W H 0.6416 0.7031 0.1814 0.043 Uiso 1 1 d R . .
O8 O 0.64377(14) 0.77510(15) 0.00175(14) 0.0351(6) Uani 1 1 d . . .
H81W H 0.6402 0.7334 -0.0176 0.042 Uiso 1 1 d R . .
H82W H 0.6423 0.8055 -0.0326 0.042 Uiso 1 1 d R . .
N1 N 0.72277(17) 0.79552(17) 0.80145(17) 0.0350(7) Uani 1 1 d . . .
O11 O 0.71311(19) 0.74566(17) 0.84609(17) 0.0521(8) Uani 1 1 d . . .
O12 O 0.7779(2) 0.85971(19) 0.80506(18) 0.0694(11) Uani 1 1 d . . .
O13 O 0.67501(18) 0.77931(17) 0.75176(19) 0.0594(9) Uani 1 1 d . . .
N2 N 0.6356(2) 0.7175(2) 0.3316(2) 0.0496(9) Uani 1 1 d . . .
O21 O 0.6723(2) 0.7530(2) 0.38610(19) 0.0617(9) Uani 1 1 d . . .
O22 O 0.5727(3) 0.7093(4) 0.3191(3) 0.1118(18) Uani 1 1 d . . .
O23 O 0.6625(2) 0.6879(2) 0.28942(19) 0.0620(9) Uani 1 1 d . . .
O1W O 0.4695(4) 0.7399(5) 0.1144(7) 0.076(3) Uani 0.41 1 d P . .
O2W O 0.4954(6) 0.7571(7) 0.2073(7) 0.082(4) Uani 0.36 1 d P . .
N3 N 0.8976(12) 1.0014(10) -0.2688(9) 0.192(11) Uani 0.40 1 d PDU A 1
O31 O 0.9191(5) 1.0314(5) -0.2036(3) 0.0442(18) Uani 0.40 1 d PD A 1
O32 O 0.9065(9) 0.9441(10) -0.3005(8) 0.130(6) Uani 0.40 1 d PD A 1
O33 O 0.8553(12) 1.0232(9) -0.3095(14) 0.45(4) Uani 0.40 1 d PD A 1
N3B N 0.9278(16) 0.9982(17) -0.2055(16) 0.098(9) Uiso 0.10 1 d PG . 2
O31B O 0.961(2) 1.0686(18) -0.200(3) 0.098(9) Uiso 0.10 1 d PG . 2
O32B O 0.9634(18) 0.964(2) -0.206(3) 0.098(9) Uiso 0.10 1 d PG . 2
O33B O 0.8571(16) 0.962(2) -0.211(3) 0.098(9) Uiso 0.10 1 d PG . 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
O O 0.0106 0.0060 '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'
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
O1 Ga1 O1 83.50(9) 2_765 10_775
O1 Ga1 O1 180.00(12) 2_765 11_565
O1 Ga1 O1 96.50(9) 10_775 11_565
O1 Ga1 O1 96.50(9) 2_765 .
O1 Ga1 O1 180.0 10_775 .
O1 Ga1 O1 83.50(9) 11_565 .
O1 Ga1 O1 96.50(9) 2_765 3_675
O1 Ga1 O1 83.50(9) 10_775 3_675
O1 Ga1 O1 83.50(9) 11_565 3_675
O1 Ga1 O1 96.50(9) . 3_675
O1 Ga1 O1 83.50(9) 2_765 12_655
O1 Ga1 O1 96.50(9) 10_775 12_655
O1 Ga1 O1 96.50(9) 11_565 12_655
O1 Ga1 O1 83.50(9) . 12_655
O1 Ga1 O1 180.0 3_675 12_655
O2 Ga2 O3 89.06(9) . .
O2 Ga2 O2 164.25(12) . 11_565
O3 Ga2 O2 96.90(9) . 11_565
O2 Ga2 O4 99.49(10) . .
O3 Ga2 O4 103.75(10) . .
O2 Ga2 O4 93.26(10) 11_565 .
O2 Ga2 O1 92.47(10) . .
O3 Ga2 O1 166.37(9) . .
O2 Ga2 O1 78.37(9) 11_565 .
O4 Ga2 O1 89.37(9) . .
O2 Ga2 O1 76.16(9) . 12_655
O3 Ga2 O1 90.68(9) . 12_655
O2 Ga2 O1 89.16(9) 11_565 12_655
O4 Ga2 O1 164.96(10) . 12_655
O1 Ga2 O1 76.57(12) . 12_655
O4 Ga3 O3 96.35(10) 12_655 .
O4 Ga3 O8 93.19(11) 12_655 .
O3 Ga3 O8 97.20(10) . .
O4 Ga3 O5 93.08(11) 12_655 .
O3 Ga3 O5 92.92(10) . .
O8 Ga3 O5 167.43(11) . .
O4 Ga3 O7 91.29(10) 12_655 .
O3 Ga3 O7 171.86(10) . .
O8 Ga3 O7 85.13(11) . .
O5 Ga3 O7 83.84(11) . .
O4 Ga3 O6 177.38(10) 12_655 .
O3 Ga3 O6 86.25(10) . .
O8 Ga3 O6 86.79(12) . .
O5 Ga3 O6 86.45(11) . .
O7 Ga3 O6 86.10(11) . .
Ga1 O1 Ga2 101.62(10) . .
Ga1 O1 Ga2 98.31(10) . 11_565
Ga2 O1 Ga2 95.47(9) . 11_565
Ga2 O2 Ga2 108.99(11) . 12_655
Ga2 O3 Ga3 134.68(12) . .
Ga3 O4 Ga2 130.90(12) 11_565 .
O12 N1 O11 121.3(3) . .
O12 N1 O13 119.7(3) . .
O11 N1 O13 119.0(3) . .
O22 N2 O21 120.8(4) . .
O22 N2 O23 119.4(5) . .
O21 N2 O23 119.8(4) . .
O31 N3 O33 117.9(12) . .
O31 N3 O32 128.1(13) . .
O33 N3 O32 113.8(11) . .
O32B N3B O31B 121.1 . .
O32B N3B O33B 119.7 . .
O31B N3B O33B 119.2 . .
O32B N3B O32B 61(3) . 3_675
O31B N3B O32B 60(3) . 3_675
O33B N3B O32B 175.2(7) . 3_675
N3B O31B O32B 61(2) . 3_675
N3B O32B O31B 123(4) . 2_765
N3B O32B O32B 61(3) . 3_675
O31B O32B O32B 174(3) 2_765 3_675
N3B O32B O32B 121(3) . 2_765
O31B O32B O32B 116(4) 2_765 2_765
O32B O32B O32B 60.0 3_675 2_765
N3B O32B N3B 179(4) . 2_765
O31B O32B N3B 58(3) 2_765 2_765
O32B O32B N3B 117(2) 3_675 2_765
O32B O32B N3B 57(2) 2_765 2_765
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ga1 O1 1.959(2) 2_765
Ga1 O1 1.959(2) 10_775
Ga1 O1 1.959(2) 11_565
Ga1 O1 1.959(2) .
Ga1 O1 1.959(2) 3_675
Ga1 O1 1.959(2) 12_655
Ga2 O2 1.910(2) .
Ga2 O3 1.913(2) .
Ga2 O2 1.917(2) 11_565
Ga2 O4 1.922(2) .
Ga2 O1 2.056(2) .
Ga2 O1 2.153(2) 12_655
Ga3 O4 1.913(2) 12_655
Ga3 O3 1.917(2) .
Ga3 O8 1.982(3) .
Ga3 O5 1.987(3) .
Ga3 O7 2.011(2) .
Ga3 O6 2.011(2) .
O1 Ga2 2.153(2) 11_565
O2 Ga2 1.917(2) 12_655
O4 Ga3 1.913(2) 11_565
N1 O12 1.218(4) .
N1 O11 1.236(4) .
N1 O13 1.247(4) .
N2 O22 1.218(5) .
N2 O21 1.239(5) .
N2 O23 1.256(5) .
O1W O2W 1.767(18) .
N3 O31 1.313(15) .
N3 O33 1.362(16) .
N3 O32 1.386(14) .
N3B O32B 1.2215 .
N3B O31B 1.2363 .
N3B O33B 1.2420 .
N3B O32B 1.28(6) 3_675
O31B O32B 1.26(7) 3_675
O32B O31B 1.26(5) 2_765
O32B O32B 1.27(5) 3_675
O32B O32B 1.27(8) 2_765
O32B N3B 1.28(5) 2_765
