#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:18:08 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179321 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/18/4321818.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_4321818
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 H36 In4 N6 O32 P8'
_chemical_formula_weight         1699.69
_chemical_name_common            '[In4(4,4'-bipy)3(HPO4)4(H2PO4)4]'
_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                112.263(1)
_cell_angle_beta                 99.093(1)
_cell_angle_gamma                102.318(1)
_cell_formula_units_Z            1
_cell_length_a                   10.4310(2)
_cell_length_b                   11.4723(2)
_cell_length_c                   11.7779(2)
_cell_measurement_reflns_used    5044
_cell_measurement_temperature    296
_cell_volume                     1229.06(4)
_computing_molecular_graphics    'ATOMS, SHELXTL version 5'
_computing_structure_refinement  'SHELXTL version 5'
_computing_structure_solution    'SHELXTL version 5'
_diffrn_ambient_temperature      296
_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  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0934
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11089
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    2.223
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.586
_exptl_crystal_colour            tan
_exptl_crystal_density_diffrn    2.296
_exptl_crystal_description       tabular
_exptl_crystal_F_000             830
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.566
_refine_diff_density_min         -1.628
_refine_diff_density_rms         0.208
_refine_ls_extinction_coef       0.0030(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.007
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         5074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_obs          0.0702
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0995P)²+1.2361P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1864
_refine_ls_wR_factor_obs         0.1661
_reflns_number_observed          3358
_reflns_number_total             5074
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9715106_2.cif
_cod_data_source_block           C30H36In4N6O32P8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0995P)^2^+1.2361P] 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^)+(0.0995P)^2^+1.2361P] 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        1229.06(5)
_cod_database_code               4321818
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 0.94567(7) 0.94480(8) 0.19915(7) 0.0396(2) Uani 1 d . .
In2 In 0.5000 0.0000 0.0000 0.0308(3) Uani 1 d S .
In3 In 0.5000 0.0000 0.5000 0.0338(3) Uani 1 d S .
P1 P 0.8031(3) -0.0106(3) -0.0534(3) 0.0422(7) Uani 1 d . .
P2 P 0.6239(3) 0.8851(3) 0.2238(3) 0.0404(7) Uani 1 d . .
P3A P 0.1555(9) 0.8339(10) 0.3656(10) 0.054(2) Uani 0.50 d P .
P3B P 0.1723(10) 0.8153(10) 0.3071(8) 0.045(2) Uani 0.50 d P .
P4 P 0.8431(7) 0.6051(4) 0.0048(4) 0.097(2) Uani 1 d . .
O1 O 0.8878(8) 0.0580(9) -0.1167(8) 0.061(2) Uani 1 d . .
O2 O 0.6650(7) 0.0080(8) -0.0798(7) 0.049(2) Uani 1 d . .
O3 O 0.8684(7) 0.0316(7) 0.0849(6) 0.043(2) Uani 1 d . .
O4 O 0.7854(10) -0.1638(9) -0.1258(8) 0.069(3) Uani 1 d . .
O5 O 0.5833(7) 0.9092(7) 0.1077(6) 0.041(2) Uani 1 d . .
O6 O 0.7786(8) 0.9380(8) 0.2806(7) 0.052(2) Uani 1 d . .
O7 O 0.5493(8) 0.9380(8) 0.3223(7) 0.048(2) Uani 1 d . .
O8 O 0.5835(9) 0.7278(8) 0.1772(8) 0.061(2) Uani 1 d . .
O9 O 0.2902(8) 0.9162(9) 0.3981(9) 0.066(2) Uani 1 d . .
O10A O 0.1579(18) 0.8333(23) 0.5069(19) 0.082(7) Uani 0.50 d P .
O10B O 0.2074(16) 0.7694(15) 0.1769(14) 0.050(4) Uani 0.50 d P .
O11 O 0.1324(11) 0.6857(10) 0.3056(14) 0.115(5) Uani 1 d . .
O12 O 0.0437(8) 0.8733(9) 0.3179(8) 0.061(2) Uani 1 d . .
O13 O 0.9003(15) 0.5608(11) 0.1034(10) 0.109(4) Uani 1 d . .
O14 O 0.6917(20) 0.5216(15) -0.0513(19) 0.229(12) Uani 1 d . .
O15 O 0.9172(29) 0.5815(22) -0.0962(19) 0.248(13) Uani 1 d . .
O16 O 0.8382(9) 0.7442(8) 0.0525(8) 0.066(2) Uani 1 d . .
N1 N 0.0543(10) 0.1544(10) 0.3542(9) 0.054(3) Uani 1 d . .
N2 N 0.6155(8) 0.2055(9) 0.1547(8) 0.040(2) Uani 1 d . .
N3 N 0.4949(9) 0.1904(8) 0.4981(8) 0.038(2) Uani 1 d . .
C1 C 0.1070(16) 0.1682(12) 0.4743(12) 0.073(4) Uani 1 d . .
C2 C 0.0633(12) 0.2599(11) 0.3311(10) 0.044(3) Uani 1 d . .
C3 C 0.1698(14) 0.2933(13) 0.5747(11) 0.062(4) Uani 1 d . .
C4 C 0.1225(10) 0.3854(12) 0.4237(10) 0.044(3) Uani 1 d . .
C5 C 0.1791(12) 0.4069(11) 0.5502(9) 0.043(3) Uani 1 d . .
C6 C 0.7517(10) 0.4601(10) 0.3475(8) 0.037(2) Uani 1 d . .
C7 C 0.6623(13) 0.4399(11) 0.2361(11) 0.053(3) Uani 1 d . .
C8 C 0.7702(12) 0.3485(12) 0.3600(10) 0.049(3) Uani 1 d . .
C9 C 0.5985(12) 0.3156(11) 0.1452(10) 0.050(3) Uani 1 d . .
C10 C 0.6992(11) 0.2231(11) 0.2627(10) 0.044(3) Uani 1 d . .
C11 C 0.4311(11) 0.1964(10) 0.3922(10) 0.039(2) Uani 1 d . .
C12 C 0.5586(11) 0.3045(10) 0.6068(10) 0.041(2) Uani 1 d . .
C13 C 0.4323(11) 0.3177(10) 0.3891(10) 0.041(2) Uani 1 d . .
C14 C 0.5645(11) 0.4278(11) 0.6089(10) 0.043(2) Uani 1 d . .
C15 C 0.4984(10) 0.4353(9) 0.4989(10) 0.035(2) 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
O12 In1 O3 173.7(3) 1_655 1_565 ?
O12 In1 O6 91.2(3) 1_655 . ?
O3 In1 O6 93.3(3) 1_565 . ?
O12 In1 O1 86.9(3) 1_655 2_765 ?
O3 In1 O1 88.8(3) 1_565 2_765 ?
O6 In1 O1 177.2(3) . 2_765 ?
O12 In1 O16 91.9(3) 1_655 . ?
O3 In1 O16 92.5(3) 1_565 . ?
O6 In1 O16 89.0(3) . . ?
O1 In1 O16 89.0(4) 2_765 . ?
O12 In1 N1 88.1(3) 1_655 1_665 ?
O3 In1 N1 87.6(3) 1_565 1_665 ?
O6 In1 N1 89.8(3) . 1_665 ?
O1 In1 N1 92.2(4) 2_765 1_665 ?
O16 In1 N1 178.8(4) . 1_665 ?
O2 In2 O2 180.0 . 2_655 ?
O2 In2 O5 90.8(3) . 1_545 ?
O2 In2 O5 89.2(3) 2_655 1_545 ?
O2 In2 O5 89.2(3) . 2_665 ?
O2 In2 O5 90.8(3) 2_655 2_665 ?
O5 In2 O5 180.0 1_545 2_665 ?
O2 In2 N2 88.2(3) . . ?
O2 In2 N2 91.8(3) 2_655 . ?
O5 In2 N2 92.0(3) 1_545 . ?
O5 In2 N2 88.0(3) 2_665 . ?
O2 In2 N2 91.8(3) . 2_655 ?
O2 In2 N2 88.2(3) 2_655 2_655 ?
O5 In2 N2 88.0(3) 1_545 2_655 ?
O5 In2 N2 92.0(3) 2_665 2_655 ?
N2 In2 N2 180.0 . 2_655 ?
O7 In3 O7 180.0 2_666 1_545 ?
O7 In3 O9 88.3(3) 2_666 2_666 ?
O7 In3 O9 91.7(3) 1_545 2_666 ?
O7 In3 O9 91.7(3) 2_666 1_545 ?
O7 In3 O9 88.3(3) 1_545 1_545 ?
O9 In3 O9 180.0 2_666 1_545 ?
O7 In3 N3 89.1(3) 2_666 . ?
O7 In3 N3 90.9(3) 1_545 . ?
O9 In3 N3 90.3(3) 2_666 . ?
O9 In3 N3 89.7(3) 1_545 . ?
O7 In3 N3 90.9(3) 2_666 2_656 ?
O7 In3 N3 89.1(3) 1_545 2_656 ?
O9 In3 N3 89.7(3) 2_666 2_656 ?
O9 In3 N3 90.3(3) 1_545 2_656 ?
N3 In3 N3 180.0 . 2_656 ?
O2 P1 O3 114.5(4) . . ?
O2 P1 O1 106.4(4) . . ?
O3 P1 O1 114.1(5) . . ?
O2 P1 O4 107.5(5) . . ?
O3 P1 O4 107.3(4) . . ?
O1 P1 O4 106.7(5) . . ?
O7 P2 O5 112.9(4) . . ?
O7 P2 O6 111.7(5) . . ?
O5 P2 O6 111.1(4) . . ?
O7 P2 O8 107.3(5) . . ?
O5 P2 O8 107.1(4) . . ?
O6 P2 O8 106.5(5) . . ?
P3B P3A O9 76.7(14) . . ?
P3B P3A O12 91.3(15) . . ?
O9 P3A O12 119.1(8) . . ?
P3B P3A O11 70.7(15) . . ?
O9 P3A O11 117.3(9) . . ?
O12 P3A O11 113.7(9) . . ?
P3B P3A O10A 154.0(19) . . ?
O9 P3A O10A 97.4(10) . . ?
O12 P3A O10A 113.2(10) . . ?
O11 P3A O10A 90.6(11) . . ?
P3B P3A O10B 1.3(12) . . ?
O9 P3A O10B 77.6(7) . . ?
O12 P3A O10B 91.6(7) . . ?
O11 P3A O10B 69.4(8) . . ?
O10A P3A O10B 153.2(10) . . ?
P3A P3B O9 74.7(14) . . ?
P3A P3B O11 82.0(14) . . ?
O9 P3B O11 121.3(9) . . ?
P3A P3B O10B 178.1(18) . . ?
O9 P3B O10B 106.6(9) . . ?
O11 P3B O10B 96.1(10) . . ?
P3A P3B O12 63.1(14) . . ?
O9 P3B O12 107.9(8) . . ?
O11 P3B O12 107.8(8) . . ?
O10B P3B O12 117.4(8) . . ?
O15 P4 O16 108.5(9) . . ?
O15 P4 O13 110.7(10) . . ?
O16 P4 O13 117.1(6) . . ?
O15 P4 O14 110.9(15) . . ?
O16 P4 O14 103.8(9) . . ?
O13 P4 O14 105.4(8) . . ?
P1 O1 In1 142.8(5) . 2_765 ?
P1 O2 In2 136.0(4) . . ?
P1 O3 In1 137.2(5) . 1_545 ?
P2 O5 In2 156.7(5) . 1_565 ?
P2 O6 In1 133.2(4) . . ?
P2 O7 In3 159.5(5) . 1_565 ?
P3A O9 P3B 28.6(4) . . ?
P3A O9 In3 155.4(7) . 1_565 ?
P3B O9 In3 155.8(7) . 1_565 ?
P3B O10B P3A 0.6(6) . . ?
P3B O11 P3A 27.3(4) . . ?
P3A O12 P3B 25.7(4) . . ?
P3A O12 In1 153.0(7) . 1_455 ?
P3B O12 In1 129.1(6) . 1_455 ?
P4 O16 In1 142.8(5) . . ?
C2 N1 C1 120.3(10) . . ?
C2 N1 In1 122.0(7) . 1_445 ?
C1 N1 In1 117.6(8) . 1_445 ?
C10 N2 C9 116.8(9) . . ?
C10 N2 In2 121.3(7) . . ?
C9 N2 In2 121.8(7) . . ?
C11 N3 C12 119.8(8) . . ?
C11 N3 In3 121.2(7) . . ?
C12 N3 In3 119.0(6) . . ?
N1 C1 C3 120.8(11) . . ?
N1 C2 C4 122.6(10) . . ?
C1 C3 C5 119.0(10) . . ?
C2 C4 C5 120.1(10) . . ?
C4 C5 C3 117.3(10) . . ?
C4 C5 C6 122.2(10) . 2_666 ?
C3 C5 C6 120.5(9) . 2_666 ?
C7 C6 C8 117.2(10) . . ?
C7 C6 C5 121.7(10) . 2_666 ?
C8 C6 C5 121.1(9) . 2_666 ?
C9 C7 C6 119.9(10) . . ?
C6 C8 C10 119.7(10) . . ?
C7 C9 N2 124.1(10) . . ?
N2 C10 C8 122.4(10) . . ?
N3 C11 C13 121.4(9) . . ?
N3 C12 C14 121.3(9) . . ?
C15 C13 C11 119.5(9) . . ?
C12 C14 C15 119.4(10) . . ?
C13 C15 C14 118.6(9) . . ?
C13 C15 C15 121.6(11) . 2_666 ?
C14 C15 C15 119.8(12) . 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 O12 2.109(7) 1_655 ?
In1 O3 2.114(6) 1_565 ?
In1 O6 2.119(8) . ?
In1 O1 2.120(8) 2_765 ?
In1 O16 2.194(9) . ?
In1 N1 2.293(10) 1_665 ?
In2 O2 2.089(7) . ?
In2 O2 2.089(7) 2_655 ?
In2 O5 2.118(6) 1_545 ?
In2 O5 2.118(6) 2_665 ?
In2 N2 2.274(9) . ?
In2 N2 2.274(9) 2_655 ?
In3 O7 2.126(7) 2_666 ?
In3 O7 2.126(7) 1_545 ?
In3 O9 2.134(8) 2_666 ?
In3 O9 2.134(8) 1_545 ?
In3 N3 2.205(8) . ?
In3 N3 2.205(8) 2_656 ?
P1 O2 1.503(7) . ?
P1 O3 1.504(7) . ?
P1 O1 1.521(8) . ?
P1 O4 1.589(9) . ?
P2 O7 1.507(7) . ?
P2 O5 1.510(6) . ?
P2 O6 1.534(8) . ?
P2 O8 1.608(9) . ?
P3A P3B 0.702(10) . ?
P3A O9 1.415(12) . ?
P3A O12 1.447(11) . ?
P3A O11 1.519(14) . ?
P3A O10A 1.66(2) . ?
P3A O10B 2.25(2) . ?
P3B O9 1.427(12) . ?
P3B O11 1.447(14) . ?
P3B O10B 1.55(2) . ?
P3B O12 1.622(13) . ?
P4 O15 1.49(2) . ?
P4 O16 1.493(9) . ?
P4 O13 1.522(11) . ?
P4 O14 1.55(2) . ?
O1 In1 2.120(8) 2_765 ?
O3 In1 2.114(6) 1_545 ?
O5 In2 2.118(6) 1_565 ?
O7 In3 2.126(7) 1_565 ?
O9 In3 2.134(8) 1_565 ?
O12 In1 2.109(7) 1_455 ?
N1 C2 1.326(13) . ?
N1 C1 1.369(14) . ?
N1 In1 2.293(10) 1_445 ?
N2 C10 1.342(13) . ?
N2 C9 1.355(13) . ?
N3 C11 1.351(12) . ?
N3 C12 1.373(13) . ?
C1 C3 1.40(2) . ?
C2 C4 1.36(2) . ?
C3 C5 1.43(2) . ?
C4 C5 1.418(14) . ?
C5 C6 1.471(14) 2_666 ?
C6 C7 1.392(14) . ?
C6 C8 1.392(15) . ?
C6 C5 1.471(14) 2_666 ?
C7 C9 1.35(2) . ?
C8 C10 1.400(15) . ?
C11 C13 1.404(13) . ?
C12 C14 1.393(14) . ?
C13 C15 1.403(14) . ?
C14 C15 1.409(13) . ?
C15 C15 1.47(2) 2_666 ?
