#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:40:23 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178819 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/73/4107361.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_4107361
loop_
_publ_author_name
'Ya-Ching Yang'
'Sue-Lein Wang'
_publ_section_title
;
 Intrinsic Yellow Light Phosphor: An Organic-Inorganic Hybrid Gallium
 Oxalatophosphate with Hexameric Octahedral Ga6(OH)4O26 Cluster
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1146
_journal_page_last               1147
_journal_paper_doi               10.1021/ja7101423
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety
'2(C13 H16 N2) Ga10 8(P O4) (H P O4) 4(O H) 2(C2 O4) 3(H2 O)'
_chemical_formula_sum            'C30 H43 Ga10 N4 O51 P9'
_chemical_formula_weight         2251.61
_chemical_name_common            NTHU6
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 132.192(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.048(3)
_cell_length_b                   24.649(3)
_cell_length_c                   17.081(3)
_cell_measurement_reflns_used    1749
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     7189.6(19)
_computing_cell_refinement       'Bruker APEX 2'
_computing_data_collection       'Bruker APEX 2'
_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      295(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'CCD area detector'
_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  0.1552
_diffrn_reflns_av_sigmaI/netI    0.1955
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33555
_diffrn_reflns_theta_full        26.88
_diffrn_reflns_theta_max         26.88
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    3.994
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.080
_exptl_crystal_description       acicular
_exptl_crystal_F_000             4416
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.937
_refine_diff_density_min         -1.903
_refine_diff_density_rms         0.572
_refine_ls_extinction_coef       0.0037(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         7478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1477
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1215P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2099
_refine_ls_wR_factor_ref         0.2493
_reflns_number_gt                3945
_reflns_number_total             7478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7101423-file004.cif
_cod_data_source_block           NTHU-6
_cod_original_cell_volume        7189.8(18)
_cod_database_code               4107361
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Ga1 Ga -0.88888(13) 1.39035(7) -1.54953(17) 0.0213(5) Uani 1 1 d .
Ga2 Ga -0.61739(13) 1.22534(8) -1.21136(15) 0.0233(5) Uani 1 1 d .
Ga3 Ga -0.79010(13) 1.26906(8) -1.45361(16) 0.0241(5) Uani 1 1 d .
Ga4 Ga -0.66435(15) 1.38278(8) -1.6201(2) 0.0341(6) Uani 1 1 d .
Ga5 Ga -0.4247(5) 1.2412(3) -1.3385(7) 0.0217(12) Uani 0.603(14) 1 d P
Ga5' Ga -0.4094(8) 1.2291(5) -1.3082(9) 0.0217(12) Uani 0.397(14) 1 d P
P1 P -0.7763(3) 1.35418(18) -1.5874(4) 0.0226(11) Uani 1 1 d .
P2 P -1.0000 1.3558(3) -1.5000 0.0205(14) Uani 1 2 d S
P3 P -0.7733(3) 1.21742(19) -1.2635(4) 0.0262(11) Uani 1 1 d .
P4 P -0.5408(3) 1.21629(19) -1.3101(4) 0.0239(11) Uani 1 1 d .
P5 P -0.5000 1.3338(3) -1.5000 0.043(2) Uani 1 2 d S
P6 P -0.6256(8) 1.5000 -1.6119(11) 0.069(3) Uani 1 2 d S
O1 O -0.8116(8) 1.3944(4) -1.5596(10) 0.028(3) Uani 1 1 d .
O2 O -0.7011(8) 1.3809(5) -1.5550(11) 0.031(3) Uani 1 1 d .
O3 O -0.7526(7) 1.3011(4) -1.5233(9) 0.022(3) Uani 1 1 d .
O4 O -0.8326(7) 1.3400(4) -1.7024(9) 0.023(3) Uani 1 1 d .
O5 O -0.9660(7) 1.3925(5) -1.5337(10) 0.026(3) Uani 1 1 d .
O6 O -1.0634(8) 1.3202(5) -1.5898(11) 0.039(4) Uani 1 1 d .
O7 O -0.6852(8) 1.2317(5) -1.1816(9) 0.031(3) Uani 1 1 d .
O8 O -0.8144(8) 1.2501(6) -1.2339(10) 0.032(3) Uani 1 1 d .
O9 O -0.8138(8) 1.2296(5) -1.3786(10) 0.028(3) Uani 1 1 d .
O10 O -0.7861(8) 1.1560(5) -1.2600(10) 0.031(3) Uani 1 1 d .
O11 O -0.5373(7) 1.2296(5) -1.2192(9) 0.021(3) Uani 1 1 d .
O12 O -0.5478(7) 1.1570(5) -1.3345(10) 0.031(3) Uani 1 1 d .
O13 O -0.4621(8) 1.2370(6) -1.2700(10) 0.037(4) Uani 1 1 d .
O14 O -0.6061(8) 1.2468(5) -1.4085(10) 0.029(3) Uani 1 1 d .
O15 O -0.8260(7) 1.3382(5) -1.4395(10) 0.024(3) Uani 1 1 d .
O16 O -0.8329(7) 1.4539(5) -1.4428(10) 0.027(3) Uani 1 1 d .
O17 O -0.5486(7) 1.2819(4) -1.0895(9) 0.024(3) Uani 1 1 d .
O18 O -0.5498(8) 1.1749(5) -1.0863(9) 0.031(3) Uani 1 1 d .
O19 O -0.6767(8) 1.2797(5) -1.3185(11) 0.034(3) Uani 1 1 d .
O20 O -0.9457(7) 1.4548(4) -1.6500(9) 0.023(3) Uani 1 1 d .
O21 O -0.4595(10) 1.2985(6) -1.3993(13) 0.055(5) Uani 1 1 d .
O22 O -0.5613(9) 1.3721(6) -1.5167(14) 0.060(5) Uani 1 1 d .
O23 O -0.6797(11) 1.4500(6) -1.6708(15) 0.066(5) Uani 1 1 d .
O24 O -0.580(3) 1.5000 -1.499(3) 0.133(17) Uani 1 2 d S
O25 O -0.569(2) 1.5000 -1.636(3) 0.110(12) Uani 1 2 d S
C1 C -0.5000 1.2601(11) -1.0000 0.030(6) Uani 1 2 d S
C2 C -0.5000 1.1980(11) -1.0000 0.025(6) Uani 1 2 d S
C3 C -0.9204(13) 1.5000 -1.6043(19) 0.015(5) Uani 1 2 d S
C4 C -0.8589(16) 1.5000 -1.489(2) 0.031(6) Uani 1 2 d S
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 0.0000 0.0000 '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'
O O 0.0106 0.0060 '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'
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
O12 Ga1 O15 99.1(5) 7_372 .
O12 Ga1 O1 92.8(6) 7_372 .
O15 Ga1 O1 89.2(5) . .
O12 Ga1 O5 91.5(6) 7_372 .
O15 Ga1 O5 92.3(5) . .
O1 Ga1 O5 175.1(5) . .
O12 Ga1 O20 89.5(5) 7_372 .
O15 Ga1 O20 171.3(5) . .
O1 Ga1 O20 89.7(5) . .
O5 Ga1 O20 88.0(5) . .
O12 Ga1 O16 169.1(5) 7_372 .
O15 Ga1 O16 91.7(5) . .
O1 Ga1 O16 88.4(5) . .
O5 Ga1 O16 86.9(5) . .
O20 Ga1 O16 79.6(4) . .
O19 Ga2 O11 89.8(6) . .
O19 Ga2 O7 90.6(6) . .
O11 Ga2 O7 168.7(5) . .
O19 Ga2 O4 100.1(5) . 7_372
O11 Ga2 O4 95.7(5) . 7_372
O7 Ga2 O4 95.3(5) . 7_372
O19 Ga2 O18 173.5(5) . .
O11 Ga2 O18 90.8(5) . .
O7 Ga2 O18 87.5(5) . .
O4 Ga2 O18 86.3(5) 7_372 .
O19 Ga2 O17 93.6(5) . .
O11 Ga2 O17 85.0(5) . .
O7 Ga2 O17 83.8(5) . .
O4 Ga2 O17 166.3(4) 7_372 .
O18 Ga2 O17 80.0(5) . .
O9 Ga3 O14 92.0(5) . 7_372
O9 Ga3 O15 91.4(5) . .
O14 Ga3 O15 92.6(5) 7_372 .
O9 Ga3 O19 91.9(6) . .
O14 Ga3 O19 172.0(6) 7_372 .
O15 Ga3 O19 94.3(5) . .
O9 Ga3 O3 171.1(5) . .
O14 Ga3 O3 91.7(5) 7_372 .
O15 Ga3 O3 96.5(5) . .
O19 Ga3 O3 83.5(5) . .
O9 Ga3 O3 94.8(5) . 7_372
O14 Ga3 O3 87.7(5) 7_372 7_372
O15 Ga3 O3 173.7(5) . 7_372
O19 Ga3 O3 85.0(5) . 7_372
O3 Ga3 O3 77.2(5) . 7_372
O22 Ga4 O23 108.3(8) . .
O22 Ga4 O2 104.6(8) . .
O23 Ga4 O2 107.6(7) . .
O22 Ga4 O10 116.7(7) . 7_372
O23 Ga4 O10 99.9(7) . 7_372
O2 Ga4 O10 119.1(6) . 7_372
O21 Ga5 O6 120.2(9) . 7_372
O21 Ga5 O13 102.3(9) . .
O6 Ga5 O13 116.4(8) 7_372 .
O21 Ga5 O8 106.3(8) . 8_575
O6 Ga5 O8 103.0(8) 7_372 8_575
O13 Ga5 O8 107.8(7) . 8_575
O8 Ga5' O13 123.9(10) 8_575 .
O8 Ga5' O6 110.4(10) 8_575 7_372
O13 Ga5' O6 123.3(10) . 7_372
O8 Ga5' O21 95.7(9) 8_575 .
O13 Ga5' O21 90.7(9) . .
O6 Ga5' O21 99.8(8) 7_372 .
O4 P1 O1 112.4(7) . .
O4 P1 O3 108.2(7) . .
O1 P1 O3 109.4(7) . .
O4 P1 O2 109.9(8) . .
O1 P1 O2 107.9(7) . .
O3 P1 O2 109.0(7) . .
O6 P2 O6 108.4(12) . 2_352
O6 P2 O5 109.5(7) . 2_352
O6 P2 O5 110.7(7) 2_352 2_352
O6 P2 O5 110.7(7) . .
O6 P2 O5 109.5(7) 2_352 .
O5 P2 O5 108.0(10) 2_352 .
O9 P3 O7 114.4(8) . .
O9 P3 O10 105.7(7) . .
O7 P3 O10 110.8(8) . .
O9 P3 O8 109.5(7) . .
O7 P3 O8 107.7(8) . .
O10 P3 O8 108.6(8) . .
O12 P4 O14 109.7(7) . .
O12 P4 O13 108.8(8) . .
O14 P4 O13 109.2(8) . .
O12 P4 O11 114.4(7) . .
O14 P4 O11 110.9(7) . .
O13 P4 O11 103.6(7) . .
O22 P5 O22 105.4(14) . 2_452
O22 P5 O21 109.8(9) . 2_452
O22 P5 O21 109.7(10) 2_452 2_452
O22 P5 O21 109.7(10) . .
O22 P5 O21 109.8(9) 2_452 .
O21 P5 O21 112.2(13) 2_452 .
O24 P6 O23 114.3(13) . .
O24 P6 O23 114.3(13) . 6_585
O23 P6 O23 105.4(16) . 6_585
O24 P6 O25 111(2) . .
O23 P6 O25 105.7(13) . .
O23 P6 O25 105.7(12) 6_585 .
P1 O1 Ga1 135.4(8) . .
P1 O2 Ga4 131.5(9) . .
P1 O3 Ga3 130.7(7) . .
P1 O3 Ga3 122.3(7) . 7_372
Ga3 O3 Ga3 102.8(5) . 7_372
P1 O4 Ga2 137.3(7) . 7_372
P2 O5 Ga1 140.2(8) . .
P2 O6 Ga5 139.9(9) . 7_372
P2 O6 Ga5' 145.7(10) . 7_372
Ga5 O6 Ga5' 15.1(3) 7_372 7_372
P3 O7 Ga2 122.9(7) . .
P3 O8 Ga5' 131.7(9) . 8_475
P3 O8 Ga5 118.2(8) . 8_475
Ga5' O8 Ga5 14.4(4) 8_475 8_475
P3 O9 Ga3 137.5(9) . .
P3 O10 Ga4 117.7(8) . 7_372
P4 O11 Ga2 130.7(8) . .
P4 O12 Ga1 139.6(8) . 7_372
P4 O13 Ga5' 135.4(10) . .
P4 O13 Ga5 130.2(9) . .
Ga5' O13 Ga5 15.0(4) . .
P4 O14 Ga3 137.7(8) . 7_372
Ga1 O15 Ga3 124.3(7) . .
C4 O16 Ga1 112.0(14) . .
C1 O17 Ga2 112.7(14) . .
C2 O18 Ga2 114.5(14) . .
Ga2 O19 Ga3 123.0(7) . .
C3 O20 Ga1 113.5(12) . .
P5 O21 Ga5 150.5(12) . .
P5 O21 Ga5' 155.6(11) . .
Ga5 O21 Ga5' 5.4(6) . .
P5 O22 Ga4 135.2(10) . .
P6 O23 Ga4 127.6(12) . .
O17 C1 O17 129(3) 2_453 .
O17 C1 C2 115.3(13) 2_453 .
O17 C1 C2 115.3(13) . .
O18 C2 O18 125(3) . 2_453
O18 C2 C1 117.3(13) . .
O18 C2 C1 117.3(13) 2_453 .
O20 C3 O20 125(2) . 6_585
O20 C3 C4 117.6(11) . .
O20 C3 C4 117.6(11) 6_585 .
O16 C4 O16 126(3) 6_585 .
O16 C4 C3 117.1(13) 6_585 .
O16 C4 C3 117.1(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ga1 O12 1.880(12) 7_372
Ga1 O15 1.904(12) .
Ga1 O1 1.905(13) .
Ga1 O5 1.970(12) .
Ga1 O20 2.041(12) .
Ga1 O16 2.069(12) .
Ga2 O19 1.911(13) .
Ga2 O11 1.942(12) .
Ga2 O7 1.948(14) .
Ga2 O4 1.952(12) 7_372
Ga2 O18 2.016(13) .
Ga2 O17 2.087(11) .
Ga3 O9 1.957(13) .
Ga3 O14 1.964(13) 7_372
Ga3 O15 1.980(11) .
Ga3 O19 2.031(14) .
Ga3 O3 2.040(12) .
Ga3 O3 2.154(11) 7_372
Ga4 O22 1.788(16) .
Ga4 O23 1.792(15) .
Ga4 O2 1.794(14) .
Ga4 O10 1.809(13) 7_372
Ga5 O21 1.611(18) .
Ga5 O6 1.849(15) 7_372
Ga5 O13 1.864(16) .
Ga5 O8 1.897(16) 8_575
Ga5' O8 1.714(19) 8_575
Ga5' O13 1.73(2) .
Ga5' O6 1.856(18) 7_372
Ga5' O21 2.07(2) .
P1 O4 1.497(12) .
P1 O1 1.544(13) .
P1 O3 1.552(12) .
P1 O2 1.567(13) .
P2 O6 1.499(14) .
P2 O6 1.499(14) 2_352
P2 O5 1.539(13) 2_352
P2 O5 1.539(13) .
P3 O9 1.538(13) .
P3 O7 1.545(15) .
P3 O10 1.550(12) .
P3 O8 1.563(14) .
P4 O12 1.497(13) .
P4 O14 1.502(13) .
P4 O13 1.534(15) .
P4 O11 1.535(13) .
P5 O22 1.557(16) .
P5 O22 1.557(16) 2_452
P5 O21 1.559(17) 2_452
P5 O21 1.559(17) .
P6 O24 1.46(3) .
P6 O23 1.549(18) .
P6 O23 1.549(18) 6_585
P6 O25 1.62(3) .
O3 Ga3 2.154(11) 7_372
O4 Ga2 1.952(12) 7_372
O6 Ga5 1.849(15) 7_372
O6 Ga5' 1.856(18) 7_372
O8 Ga5' 1.714(19) 8_475
O8 Ga5 1.897(16) 8_475
O10 Ga4 1.809(13) 7_372
O12 Ga1 1.880(12) 7_372
O14 Ga3 1.964(13) 7_372
O16 C4 1.278(17) .
O17 C1 1.258(16) .
O18 C2 1.242(16) .
O20 C3 1.257(15) .
C1 O17 1.258(16) 2_453
C1 C2 1.53(4) .
C2 O18 1.242(16) 2_453
C3 O20 1.257(15) 6_585
C3 C4 1.47(3) .
C4 O16 1.278(17) 6_585
