#------------------------------------------------------------------------------
#$Date: 2019-11-22 23:51:39 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231601 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/60/4346053.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_4346053
loop_
_publ_author_name
'Kamunde-Devonish, Maisha K'
'Fast, Dylan B.'
'Mensinger, Zachary L.'
'Gatlin, Jason T.'
'Zakharov, Lev N.'
'Dolgos, Michelle R.'
'Johnson, Darren W.'
_publ_section_title
;
 Synthesis and solid-state structural characterization of a series of
 aqueous heterometallic tridecameric group 13 clusters.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3913
_journal_page_last               3920
_journal_paper_doi               10.1021/acs.inorgchem.5b00097
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C6 H96 Ga10.27 In2.73 N15 O99'
_chemical_formula_weight         2992.46
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_cell_setting           trigonal
_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           SHELXLTL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   20.2946(12)
_cell_length_b                   20.2946(12)
_cell_length_c                   18.456(2)
_cell_measurement_reflns_used    6442
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.49
_cell_volume                     6583.1(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex CCD'
_diffrn_measurement_method       'phi and omega 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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13370
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    3.955
_exptl_absorpt_correction_T_max  0.8268
_exptl_absorpt_correction_T_min  0.6931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             4443
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0419P)²+19.2722P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0732
_reflns_number_gt                2938
_reflns_number_total             3195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00097_si_002.cif
_cod_data_source_block           jtg65_sqd
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Trigonal' was changed to
'trigonal' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        6583.2(9)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4346053
_platon_squeeze_void_probe_radius 1.20
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
Ga1 Ga 0.3333 0.6667 0.1667 0.01542(16) Uani 1 6 d S
Ga2 Ga 0.475953(16) 0.829241(16) 0.162950(15) 0.01597(11) Uani 1 1 d .
Ga3 Ga 0.638332(13) 0.848029(13) 0.072436(13) 0.01897(10) Uani 0.564(5) 1 d P
In3 In 0.638332(13) 0.848029(13) 0.072436(13) 0.01897(10) Uani 0.436(5) 1 d P
O1 O 0.42875(10) 0.72488(10) 0.11271(10) 0.0167(4) Uani 1 1 d .
O2 O 0.40702(10) 0.85482(11) 0.11729(10) 0.0187(4) Uani 1 1 d .
O3 O 0.55488(11) 0.87182(11) 0.09118(10) 0.0214(4) Uani 1 1 d .
O5 O 0.70702(13) 0.95568(13) 0.02899(12) 0.0309(5) Uani 1 1 d .
O6 O 0.69355(13) 0.89779(14) 0.16809(12) 0.0349(5) Uani 1 1 d .
O7 O 0.60455(13) 0.81769(13) -0.03458(13) 0.0336(5) Uani 1 1 d .
O8 O 0.72625(15) 0.82647(14) 0.05173(14) 0.0385(6) Uani 1 1 d .
O9 O 0.57879(11) 0.73926(11) 0.10463(10) 0.0217(4) Uani 1 1 d .
N1S N 0.40680(15) 0.94309(15) -0.03231(13) 0.0272(5) Uani 1 1 d .
O1S O 0.41813(19) 0.88904(17) -0.02630(14) 0.0545(8) Uani 1 1 d .
O2S O 0.36441(15) 0.95196(14) 0.01032(13) 0.0396(6) Uani 1 1 d .
O3S O 0.43802(17) 0.98914(15) -0.08242(16) 0.0506(7) Uani 1 1 d .
N2S N 0.74950(19) 0.69975(19) 0.16280(17) 0.0432(7) Uani 1 1 d .
O4S O 0.8034(2) 0.7626(2) 0.1512(2) 0.0774(11) Uani 1 1 d .
O5S O 0.69257(16) 0.67297(18) 0.12160(14) 0.0516(7) Uani 1 1 d .
O6S O 0.74911(16) 0.66072(18) 0.21597(14) 0.0505(7) Uani 1 1 d .
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'
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'
In In -0.7276 1.3100 '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 180.0 14_455 2_665
O1 Ga1 O1 96.52(7) 14_455 13_565
O1 Ga1 O1 83.48(7) 2_665 13_565
O1 Ga1 O1 83.48(7) 14_455 .
O1 Ga1 O1 96.52(7) 2_665 .
O1 Ga1 O1 180.0 13_565 .
O1 Ga1 O1 96.52(7) 14_455 15
O1 Ga1 O1 83.48(7) 2_665 15
O1 Ga1 O1 96.52(7) 13_565 15
O1 Ga1 O1 83.48(7) . 15
O1 Ga1 O1 83.48(7) 14_455 3_565
O1 Ga1 O1 96.53(7) 2_665 3_565
O1 Ga1 O1 83.48(7) 13_565 3_565
O1 Ga1 O1 96.52(7) . 3_565
O1 Ga1 O1 180.0 15 3_565
O9 Ga2 O2 89.86(8) 15 .
O9 Ga2 O2 95.70(8) 15 14_455
O2 Ga2 O2 165.41(10) . 14_455
O9 Ga2 O3 102.34(9) 15 .
O2 Ga2 O3 97.63(8) . .
O2 Ga2 O3 94.35(8) 14_455 .
O9 Ga2 O1 166.46(8) 15 .
O2 Ga2 O1 93.07(8) . .
O2 Ga2 O1 78.51(8) 14_455 .
O3 Ga2 O1 90.38(8) . .
O9 Ga2 O1 91.34(8) 15 15
O2 Ga2 O1 76.12(7) . 15
O2 Ga2 O1 90.25(8) 14_455 15
O3 Ga2 O1 165.03(8) . 15
O1 Ga2 O1 76.57(10) . 15
O9 Ga3 O3 95.58(8) . .
O9 Ga3 O6 99.56(9) . .
O3 Ga3 O6 92.97(9) . .
O9 Ga3 O8 86.03(9) . .
O3 Ga3 O8 178.38(9) . .
O6 Ga3 O8 86.96(10) . .
O9 Ga3 O5 172.19(8) . .
O3 Ga3 O5 90.96(8) . .
O6 Ga3 O5 84.31(9) . .
O8 Ga3 O5 87.42(9) . .
O9 Ga3 O7 91.57(9) . .
O3 Ga3 O7 92.40(9) . .
O6 Ga3 O7 167.10(9) . .
O8 Ga3 O7 87.34(10) . .
O5 Ga3 O7 83.88(9) . .
Ga1 O1 Ga2 101.68(8) . .
Ga1 O1 Ga2 98.27(8) . 14_455
Ga2 O1 Ga2 95.47(7) . 14_455
Ga2 O2 Ga2 109.11(9) . 15
Ga2 O3 Ga3 128.66(10) . .
Ga2 O9 Ga3 132.97(11) 14_455 .
O1S N1S O3S 119.0(3) . .
O1S N1S O2S 121.5(3) . .
O3S N1S O2S 119.5(3) . .
O4S N2S O5S 119.8(4) . .
O4S N2S O6S 121.2(4) . .
O5S N2S O6S 119.0(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ga1 O1 1.9619(18) 14_455
Ga1 O1 1.9620(18) 2_665
Ga1 O1 1.9620(18) 13_565
Ga1 O1 1.9620(18) .
Ga1 O1 1.9620(18) 15
Ga1 O1 1.9621(18) 3_565
Ga2 O9 1.9097(19) 15
Ga2 O2 1.9138(18) .
Ga2 O2 1.9155(18) 14_455
Ga2 O3 1.9191(19) .
Ga2 O1 2.0578(18) .
Ga2 O1 2.1567(18) 15
Ga3 O9 2.005(2) .
Ga3 O3 2.0096(19) .
Ga3 O6 2.064(2) .
Ga3 O8 2.074(2) .
Ga3 O5 2.077(2) .
Ga3 O7 2.080(2) .
O1 Ga2 2.1566(18) 14_455
O2 Ga2 1.9157(18) 15
O9 Ga2 1.9097(19) 14_455
N1S O1S 1.233(4) .
N1S O3S 1.240(3) .
N1S O2S 1.244(3) .
N2S O4S 1.215(5) .
N2S O5S 1.257(4) .
N2S O6S 1.259(4) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 546 197 ' '
2 0.667 0.333 0.333 546 197 ' '
3 0.333 0.667 0.667 545 197 ' '
