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#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/80/2228058.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_2228058
loop_
_publ_author_name
'Assani, Abderrazzak'
'Saadi, Mohamed'
'El Ammari, Lahcen'
_publ_section_title
;
 A one-dimensional inorganic--organic hybrid compound:
 catena-poly[ethylenediammonium
 [indate(III)-di-μ-hydrogenphosphato(V)-μ-hydroxido] monohydrate]
;
_journal_coeditor_code           WM2383
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1065
_journal_page_last               m1066
_journal_paper_doi               10.1107/S160053681003240X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(C2 H10 N2) [In (H P O4)2 (O H)], H2 O'
_chemical_formula_moiety         'C2 H10 N2 2+, H3 In O9 P2 2-, H2 O'
_chemical_formula_sum            'C2 H15 In N2 O10 P2'
_chemical_formula_weight         403.92
_chemical_name_systematic
;
catena-poly[ethylenediammonium
[indate(III)-di-μ-hydrogenphosphato(V)-μ-hydroxido] monohydrate]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 99.0000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0702(3)
_cell_length_b                   7.4896(2)
_cell_length_c                   15.6007(5)
_cell_measurement_reflns_used    2771
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.61
_cell_volume                     1162.15(6)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8 APEXII CCD area-detector'
_diffrn_measurement_method       'φ and 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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13591
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.61
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.357
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.652
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2771
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0258
_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)+(0.0310P)²+0.4367P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0671
_reflns_number_gt                2168
_reflns_number_total             2771
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm2383.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2228058
_cod_database_fobs_code          2228058
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
In In1 0.247040(19) 0.02859(3) 0.250039(14) 0.01340(8) Uani d . 1 . .
P P1 0.12174(8) -0.22253(11) 0.39952(5) 0.01587(17) Uani d . 1 . .
P P2 -0.02212(8) -0.22671(10) 0.15538(5) 0.01537(17) Uani d . 1 . .
O O1 -0.0298(2) -0.2219(4) 0.37808(17) 0.0389(7) Uani d . 1 . .
O O2 0.1861(2) -0.3858(3) 0.36661(15) 0.0271(5) Uani d . 1 . .
O O3 0.1849(2) -0.0520(3) 0.36984(15) 0.0271(6) Uani d . 1 . .
O O4 0.1498(2) -0.2250(3) 0.50197(14) 0.0235(5) Uani d . 1 . .
H H4 0.2297 -0.2449 0.5186 0.035 Uiso calc R 1 . .
O O5 -0.0986(2) -0.2250(3) 0.06416(15) 0.0233(5) Uani d . 1 . .
O O6 0.0672(2) -0.3905(3) 0.17185(15) 0.0246(5) Uani d . 1 . .
O O7 0.0595(2) -0.0564(3) 0.17533(16) 0.0243(5) Uani d . 1 . .
O O8 -0.1324(2) -0.2335(4) 0.21683(17) 0.0366(7) Uani d . 1 . .
H H8 -0.0965 -0.2205 0.2673 0.055 Uiso calc R 1 . .
O O9 0.3367(2) -0.2199(3) 0.23619(15) 0.0174(5) Uani d D 1 . .
H H9 0.4156(15) -0.208(4) 0.222(2) 0.026 Uiso d D 1 . .
O O10 0.5844(4) -0.1357(6) 0.1893(3) 0.0634(14) Uani d P 0.70 . .
H H10A 0.5706 -0.0285 0.1724 0.095 Uiso d R 1 . .
H H10B 0.6316 -0.2340 0.1945 0.095 Uiso d R 1 . .
O O11 0.5872(10) -0.3060(14) 0.2029(9) 0.0634(14) Uani d P 0.30 . .
N N1 0.3639(3) -0.2375(4) 0.0340(2) 0.0309(7) Uani d . 1 . .
H H11A 0.3562 -0.3278 0.0701 0.046 Uiso calc R 1 . .
H H11B 0.4083 -0.1482 0.0633 0.046 Uiso calc R 1 . .
H H11C 0.4086 -0.2738 -0.0076 0.046 Uiso calc R 1 . .
N N2 0.0128(3) -0.2744(4) -0.0842(2) 0.0281(7) Uani d . 1 . .
H H22A -0.0222 -0.2442 -0.0372 0.042 Uiso calc R 1 . .
H H22B -0.0317 -0.3677 -0.1098 0.042 Uiso calc R 1 . .
H H22C 0.0059 -0.1828 -0.1209 0.042 Uiso calc R 1 . .
C C1 0.2296(3) -0.1762(5) -0.0048(2) 0.0276(8) Uani d . 1 . .
H H1A 0.2376 -0.0727 -0.0410 0.033 Uiso calc R 1 . .
H H1B 0.1792 -0.1414 0.0406 0.033 Uiso calc R 1 . .
C C2 0.1563(3) -0.3220(5) -0.0585(2) 0.0300(8) Uani d . 1 . .
H H2A 0.1972 -0.3411 -0.1101 0.036 Uiso calc R 1 . .
H H2B 0.1632 -0.4322 -0.0254 0.036 Uiso calc R 1 . .
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O9 In1 O9 2 . 178.25(5) ?
O9 In1 O2 2 2 90.18(9) ?
O9 In1 O2 . 2 88.87(9) ?
O9 In1 O3 2 . 89.24(8) ?
O9 In1 O3 . . 91.66(8) ?
O2 In1 O3 2 . 178.07(9) ?
O9 In1 O6 2 2 90.97(8) ?
O9 In1 O6 . 2 87.60(8) ?
O2 In1 O6 2 2 92.06(9) ?
O3 In1 O6 . 2 86.11(9) ?
O9 In1 O7 2 . 89.32(8) ?
O9 In1 O7 . . 92.14(8) ?
O2 In1 O7 2 . 89.67(9) ?
O3 In1 O7 . . 92.16(9) ?
O6 In1 O7 2 . 178.24(9) ?
O1 P1 O2 . . 113.55(15) ?
O1 P1 O3 . . 112.56(15) ?
O2 P1 O3 . . 110.60(13) ?
O1 P1 O4 . . 103.80(13) ?
O2 P1 O4 . . 108.44(13) ?
O3 P1 O4 . . 107.41(14) ?
O5 P2 O6 . . 111.58(13) ?
O5 P2 O7 . . 111.43(13) ?
O6 P2 O7 . . 110.81(13) ?
O5 P2 O8 . . 105.63(14) ?
O6 P2 O8 . . 109.01(15) ?
O7 P2 O8 . . 108.16(14) ?
P1 O2 In1 . 2_545 137.89(14) ?
P1 O3 In1 . . 133.57(14) ?
P1 O4 H4 . . 109.5 ?
P2 O6 In1 . 2_545 139.63(14) ?
P2 O7 In1 . . 139.23(14) ?
P2 O8 H8 . . 109.5 ?
In1 O9 In1 2_545 . 127.09(10) ?
In1 O9 H9 2_545 . 122(2) ?
In1 O9 H9 . . 111(2) ?
O11 O10 H10A . . 169.0 ?
O11 O10 H10B . . 32.4 ?
H10A O10 H10B . . 152.4 ?
O10 O11 H10B . . 40.1 ?
C1 N1 H11A . . 109.5 ?
C1 N1 H11B . . 109.5 ?
H11A N1 H11B . . 109.5 ?
C1 N1 H11C . . 109.5 ?
H11A N1 H11C . . 109.5 ?
H11B N1 H11C . . 109.5 ?
C2 N2 H22A . . 109.5 ?
C2 N2 H22B . . 109.5 ?
H22A N2 H22B . . 109.5 ?
C2 N2 H22C . . 109.5 ?
H22A N2 H22C . . 109.5 ?
H22B N2 H22C . . 109.5 ?
N1 C1 C2 . . 110.2(3) ?
N1 C1 H1A . . 109.6 ?
C2 C1 H1A . . 109.6 ?
N1 C1 H1B . . 109.6 ?
C2 C1 H1B . . 109.6 ?
H1A C1 H1B . . 108.1 ?
N2 C2 C1 . . 110.5(3) ?
N2 C2 H2A . . 109.5 ?
C1 C2 H2A . . 109.5 ?
N2 C2 H2B . . 109.5 ?
C1 C2 H2B . . 109.5 ?
H2A C2 H2B . . 108.1 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
In1 O9 2 2.089(2) y
In1 O9 . 2.094(2) y
In1 O2 2 2.135(2) y
In1 O3 . 2.148(2) y
In1 O6 2 2.154(2) y
In1 O7 . 2.154(2) y
P1 O1 . 1.510(3) ?
P1 O2 . 1.511(2) ?
P1 O3 . 1.530(2) ?
P1 O4 . 1.579(2) ?
P2 O5 . 1.509(2) ?
P2 O6 . 1.519(2) ?
P2 O7 . 1.523(2) ?
P2 O8 . 1.577(3) ?
O2 In1 2_545 2.135(2) ?
O4 H4 . 0.8200 ?
O6 In1 2_545 2.154(2) ?
O8 H8 . 0.8200 ?
O9 In1 2_545 2.089(2) ?
O9 H9 . 0.862(17) ?
O10 O11 . 1.293(12) ?
O10 H10A . 0.8496 ?
O10 H10B . 0.8728 ?
O11 H10B . 0.7256 ?
N1 C1 . 1.466(4) ?
N1 H11A . 0.8900 ?
N1 H11B . 0.8900 ?
N1 H11C . 0.8900 ?
N2 C2 . 1.481(4) ?
N2 H22A . 0.8900 ?
N2 H22B . 0.8900 ?
N2 H22C . 0.8900 ?
C1 C2 . 1.498(5) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O4 H4 O5 4_656 0.82 1.78 2.595(3) 174
O8 H8 O1 . 0.82 1.75 2.567(4) 172
O9 H9 O10 . 0.862(17) 1.93(2) 2.780(5) 170(3)
O10 H10A O1 2_555 0.85 2.44 3.291(5) 179
O10 H10B O8 1_655 0.87 2.35 2.911(5) 122
N1 H11A O3 2_545 0.89 2.00 2.876(4) 168
N1 H11B O2 2_555 0.89 2.51 3.137(4) 128
N1 H11B O10 . 0.89 2.43 3.114(5) 133
N1 H11C O4 4_655 0.89 2.41 3.011(4) 125
N1 H11C O1 4_655 0.89 1.98 2.823(4) 158
N2 H22A O5 . 0.89 1.87 2.750(4) 170
N2 H22B O6 3_545 0.89 2.06 2.911(4) 160
N2 H22C O7 3_555 0.89 2.05 2.892(4) 158
