#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:18:08 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179321 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/18/4321817.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_4321817
loop_
_publ_author_name
'Kwang-Hwa Lii'
'Yuh-Feng Huang'
_publ_section_title
;
 Synthesis and Structures of [In4(4,4'-bipy)3(HPO4)4(H2PO4)4].4H2O and
 In4(4,4'-bipy)3(HPO4)4(H2PO4)4, Indium Phosphates with a Pillared Layer
 Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1348
_journal_page_last               1350
_journal_paper_doi               10.1021/ic9715106
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C30 H44 In4 N6 O36 P8'
_chemical_formula_weight         1771.75
_chemical_name_common            '[In4(4,4'-bipy)3(HPO4)4(H2PO4)4].4H2O'
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                110.116(1)
_cell_angle_beta                 100.445(1)
_cell_angle_gamma                104.339(1)
_cell_formula_units_Z            1
_cell_length_a                   10.5429(4)
_cell_length_b                   11.6345(5)
_cell_length_c                   11.7303(5)
_cell_measurement_reflns_used    5375
_cell_measurement_temperature    296
_cell_volume                     1251.58(9)
_computing_molecular_graphics    'ATOMS, SHELXTL version 5'
_computing_structure_refinement  'SHELXTL version 5'
_computing_structure_solution    'SHELXTL version 5'
_diffrn_ambient_temperature      296
_diffrn_measurement_device       'Siemens Smart CCD'
_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  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0881
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12334
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    2.194
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.761
_exptl_crystal_colour            tan
_exptl_crystal_density_diffrn    2.351
_exptl_crystal_description       tabular
_exptl_crystal_F_000             870
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.160
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.204
_refine_ls_extinction_coef       0.0024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.048
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         5678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_obs          0.0517
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0426P)²+3.6157P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1163
_refine_ls_wR_factor_obs         0.1034
_reflns_number_observed          4045
_reflns_number_total             5678
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9715106_1.cif
_cod_data_source_block           C30H44In4N6O36P8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+3.6157P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+3.6157P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1251.58(15)
_cod_database_code               4321817
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
In1 In 0.95369(5) 0.95538(5) 0.20526(5) 0.01270(14) Uani 1 d . .
In2 In 0.5000 0.0000 0.0000 0.0099(2) Uani 1 d S .
In3 In 0.5000 0.0000 0.5000 0.0119(2) Uani 1 d S .
P1 P 0.8064(2) 0.0026(2) -0.0498(2) 0.0135(4) Uani 1 d . .
P2 P 0.6324(2) 0.9023(2) 0.2365(2) 0.0140(4) Uani 1 d . .
P3 P 0.1546(2) 0.8379(2) 0.3667(2) 0.0156(4) Uani 1 d . .
P4 P 0.8016(3) 0.6226(2) 0.0232(2) 0.0398(6) Uani 1 d . .
O1 O 0.8787(5) 0.0423(5) 0.0890(4) 0.0183(11) Uani 1 d . .
O2 O 0.8924(5) 0.0679(5) -0.1153(5) 0.0248(12) Uani 1 d . .
O3 O 0.6722(4) 0.0315(5) -0.0679(5) 0.0205(11) Uani 1 d . .
O4 O 0.7727(6) -0.1502(5) -0.1203(5) 0.0301(13) Uani 1 d . .
O5 O 0.7889(5) 0.9590(5) 0.2939(5) 0.0224(12) Uani 1 d . .
O6 O 0.5893(5) 0.9188(5) 0.1152(4) 0.0170(10) Uani 1 d . .
O7 O 0.5646(5) 0.9601(5) 0.3335(5) 0.0245(12) Uani 1 d . .
O8 O 0.5859(6) 0.7497(5) 0.1994(5) 0.0329(14) Uani 1 d . .
O9 O 0.0407(5) 0.8893(5) 0.3357(4) 0.0181(11) Uani 1 d . .
O10 O 0.2947(5) 0.9215(5) 0.3801(5) 0.0207(11) Uani 1 d . .
O11 O 0.1549(5) 0.8188(5) 0.4939(5) 0.0271(13) Uani 1 d . .
O12 O 0.1230(5) 0.6988(5) 0.2632(5) 0.0343(14) Uani 1 d . .
O13 O 0.8830(8) 0.5880(6) 0.1159(7) 0.072(3) Uani 1 d . .
O14 O 0.8248(6) 0.7644(5) 0.0666(5) 0.0339(14) Uani 1 d . .
O15 O 0.8141(10) 0.5672(9) -0.1115(6) 0.098(4) Uani 1 d . .
O16 O 0.6459(8) 0.5548(8) -0.0017(9) 0.101(4) Uani 1 d . .
N1 N 0.0699(6) 0.1592(6) 0.3582(5) 0.0187(13) Uani 1 d . .
N2 N 0.6044(6) 0.2058(5) 0.1541(5) 0.0157(13) Uani 1 d . .
N3 N 0.5045(6) 0.1955(5) 0.5010(6) 0.0158(13) Uani 1 d . .
C1 C 0.1278(7) 0.1768(7) 0.4784(7) 0.019(2) Uani 1 d . .
C2 C 0.0723(7) 0.2646(7) 0.3348(7) 0.019(2) Uani 1 d . .
C3 C 0.1899(7) 0.3005(7) 0.5765(7) 0.018(2) Uani 1 d . .
C4 C 0.1314(7) 0.3912(7) 0.4280(7) 0.020(2) Uani 1 d . .
C5 C 0.1933(7) 0.4097(7) 0.5545(7) 0.018(2) Uani 1 d . .
C6 C 0.7392(7) 0.4580(7) 0.3454(6) 0.016(2) Uani 1 d . .
C7 C 0.6351(7) 0.4329(7) 0.2352(7) 0.020(2) Uani 1 d . .
C8 C 0.7730(7) 0.3529(7) 0.3531(7) 0.019(2) Uani 1 d . .
C9 C 0.5707(7) 0.3077(7) 0.1444(7) 0.018(2) Uani 1 d . .
C10 C 0.7072(7) 0.2286(7) 0.2560(7) 0.023(2) Uani 1 d . .
C11 C 0.4315(7) 0.2015(7) 0.3952(7) 0.0174(15) Uani 1 d . .
C12 C 0.5746(7) 0.3084(7) 0.6058(7) 0.018(2) Uani 1 d . .
C13 C 0.4299(7) 0.3192(6) 0.3926(6) 0.0152(15) Uani 1 d . .
C14 C 0.5743(7) 0.4273(7) 0.6073(7) 0.0171(15) Uani 1 d . .
C15 C 0.5007(6) 0.4355(6) 0.4999(6) 0.0126(14) Uani 1 d . .
OW1 O 0.7016(7) 0.2744(7) 0.8997(7) 0.056(2) Uani 1 d . .
OW2 O 0.9399(9) 0.3747(8) 0.1204(9) 0.089(3) Uani 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'
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'
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
_geom_angle_publ_flag
O9 In1 O1 173.8(2) 1_655 1_565 ?
O9 In1 O2 89.5(2) 1_655 2_765 ?
O1 In1 O2 91.1(2) 1_565 2_765 ?
O9 In1 O14 95.0(2) 1_655 . ?
O1 In1 O14 91.2(2) 1_565 . ?
O2 In1 O14 87.8(2) 2_765 . ?
O9 In1 O5 87.7(2) 1_655 . ?
O1 In1 O5 92.2(2) 1_565 . ?
O2 In1 O5 174.4(2) 2_765 . ?
O14 In1 O5 87.6(2) . . ?
O9 In1 N1 86.0(2) 1_655 1_665 ?
O1 In1 N1 87.8(2) 1_565 1_665 ?
O2 In1 N1 98.2(2) 2_765 1_665 ?
O14 In1 N1 173.9(2) . 1_665 ?
O5 In1 N1 86.5(2) . 1_665 ?
O3 In2 O3 180.0 2_655 . ?
O3 In2 O6 88.6(2) 2_655 1_545 ?
O3 In2 O6 91.4(2) . 1_545 ?
O3 In2 O6 91.4(2) 2_655 2_665 ?
O3 In2 O6 88.6(2) . 2_665 ?
O6 In2 O6 180.0 1_545 2_665 ?
O3 In2 N2 87.0(2) 2_655 2_655 ?
O3 In2 N2 93.0(2) . 2_655 ?
O6 In2 N2 87.8(2) 1_545 2_655 ?
O6 In2 N2 92.2(2) 2_665 2_655 ?
O3 In2 N2 93.0(2) 2_655 . ?
O3 In2 N2 87.0(2) . . ?
O6 In2 N2 92.2(2) 1_545 . ?
O6 In2 N2 87.8(2) 2_665 . ?
N2 In2 N2 180.0 2_655 . ?
O7 In3 O7 180.0 1_545 2_666 ?
O7 In3 O10 92.2(2) 1_545 2_666 ?
O7 In3 O10 87.8(2) 2_666 2_666 ?
O7 In3 O10 87.8(2) 1_545 1_545 ?
O7 In3 O10 92.2(2) 2_666 1_545 ?
O10 In3 O10 180.0 2_666 1_545 ?
O7 In3 N3 91.4(2) 1_545 2_656 ?
O7 In3 N3 88.6(2) 2_666 2_656 ?
O10 In3 N3 88.1(2) 2_666 2_656 ?
O10 In3 N3 91.9(2) 1_545 2_656 ?
O7 In3 N3 88.6(2) 1_545 . ?
O7 In3 N3 91.4(2) 2_666 . ?
O10 In3 N3 91.9(2) 2_666 . ?
O10 In3 N3 88.1(2) 1_545 . ?
N3 In3 N3 180.0 2_656 . ?
O2 P1 O1 113.6(3) . . ?
O2 P1 O3 107.3(3) . . ?
O1 P1 O3 112.2(3) . . ?
O2 P1 O4 107.8(3) . . ?
O1 P1 O4 107.2(3) . . ?
O3 P1 O4 108.5(3) . . ?
O6 P2 O7 113.2(3) . . ?
O6 P2 O5 110.9(3) . . ?
O7 P2 O5 110.1(3) . . ?
O6 P2 O8 106.4(3) . . ?
O7 P2 O8 107.7(3) . . ?
O5 P2 O8 108.2(3) . . ?
O10 P3 O9 114.9(3) . . ?
O10 P3 O12 108.8(3) . . ?
O9 P3 O12 109.8(3) . . ?
O10 P3 O11 109.3(3) . . ?
O9 P3 O11 108.5(3) . . ?
O12 P3 O11 105.1(3) . . ?
O13 P4 O14 114.0(4) . . ?
O13 P4 O15 114.7(5) . . ?
O14 P4 O15 110.1(5) . . ?
O13 P4 O16 109.7(5) . . ?
O14 P4 O16 106.6(5) . . ?
O15 P4 O16 100.6(6) . . ?
P1 O1 In1 138.0(3) . 1_545 ?
P1 O2 In1 139.4(3) . 2_765 ?
P1 O3 In2 135.8(3) . . ?
P2 O5 In1 131.4(3) . . ?
P2 O6 In2 155.0(3) . 1_565 ?
P2 O7 In3 158.7(3) . 1_565 ?
P3 O9 In1 142.0(3) . 1_455 ?
P3 O10 In3 141.3(3) . 1_565 ?
P4 O14 In1 144.9(3) . . ?
C2 N1 C1 118.3(6) . . ?
C2 N1 In1 121.1(5) . 1_445 ?
C1 N1 In1 120.3(5) . 1_445 ?
C9 N2 C10 118.6(6) . . ?
C9 N2 In2 121.7(5) . . ?
C10 N2 In2 119.6(5) . . ?
C12 N3 C11 118.7(6) . . ?
C12 N3 In3 121.8(4) . . ?
C11 N3 In3 119.5(4) . . ?
N1 C1 C3 121.7(7) . . ?
N1 C2 C4 123.3(7) . . ?
C5 C3 C1 120.9(7) . . ?
C2 C4 C5 118.3(7) . . ?
C3 C5 C4 117.4(6) . . ?
C3 C5 C6 122.6(6) . 2_666 ?
C4 C5 C6 120.0(6) . 2_666 ?
C8 C6 C7 116.9(6) . . ?
C8 C6 C5 122.2(6) . 2_666 ?
C7 C6 C5 120.9(6) . 2_666 ?
C9 C7 C6 119.9(7) . . ?
C6 C8 C10 120.7(7) . . ?
N2 C9 C7 122.4(7) . . ?
N2 C10 C8 121.5(7) . . ?
N3 C11 C13 121.3(6) . . ?
N3 C12 C14 121.7(6) . . ?
C11 C13 C15 120.5(6) . . ?
C12 C14 C15 120.4(6) . . ?
C13 C15 C14 117.4(6) . . ?
C13 C15 C15 121.6(7) . 2_666 ?
C14 C15 C15 121.0(8) . 2_666 ?
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
In1 O9 2.103(5) 1_655 ?
In1 O1 2.112(5) 1_565 ?
In1 O2 2.112(5) 2_765 ?
In1 O14 2.156(5) . ?
In1 O5 2.183(5) . ?
In1 N1 2.276(6) 1_665 ?
In2 O3 2.112(4) 2_655 ?
In2 O3 2.112(4) . ?
In2 O6 2.113(5) 1_545 ?
In2 O6 2.113(5) 2_665 ?
In2 N2 2.282(5) 2_655 ?
In2 N2 2.282(5) . ?
In3 O7 2.123(5) 1_545 ?
In3 O7 2.123(5) 2_666 ?
In3 O10 2.129(5) 2_666 ?
In3 O10 2.129(5) 1_545 ?
In3 N3 2.260(6) 2_656 ?
In3 N3 2.260(6) . ?
P1 O2 1.517(5) . ?
P1 O1 1.518(5) . ?
P1 O3 1.529(5) . ?
P1 O4 1.593(5) . ?
P2 O6 1.504(5) . ?
P2 O7 1.505(5) . ?
P2 O5 1.537(5) . ?
P2 O8 1.595(5) . ?
P3 O10 1.501(5) . ?
P3 O9 1.510(5) . ?
P3 O12 1.562(5) . ?
P3 O11 1.581(5) . ?
P4 O13 1.489(7) . ?
P4 O14 1.489(6) . ?
P4 O15 1.532(8) . ?
P4 O16 1.558(8) . ?
O1 In1 2.112(5) 1_545 ?
O2 In1 2.112(5) 2_765 ?
O6 In2 2.113(5) 1_565 ?
O7 In3 2.123(5) 1_565 ?
O9 In1 2.103(5) 1_455 ?
O10 In3 2.129(4) 1_565 ?
N1 C2 1.341(9) . ?
N1 C1 1.353(9) . ?
N1 In1 2.276(6) 1_445 ?
N2 C9 1.353(9) . ?
N2 C10 1.357(9) . ?
N3 C12 1.364(9) . ?
N3 C11 1.370(9) . ?
C1 C3 1.395(9) . ?
C2 C4 1.395(10) . ?
C3 C5 1.374(10) . ?
C4 C5 1.426(10) . ?
C5 C6 1.472(9) 2_666 ?
C6 C8 1.383(10) . ?
C6 C7 1.424(9) . ?
C6 C5 1.472(9) 2_666 ?
C7 C9 1.377(9) . ?
C8 C10 1.397(10) . ?
C11 C13 1.385(9) . ?
C12 C14 1.379(9) . ?
C13 C15 1.400(9) . ?
C14 C15 1.401(9) . ?
C15 C15 1.504(13) 2_666 ?
