#------------------------------------------------------------------------------
#$Date: 2015-08-08 04:53:39 +0300 (Sat, 08 Aug 2015) $
#$Revision: 153145 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/56/7035619.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_7035619
loop_
_publ_author_name
'Luan, Lindong'
'Yang, Meng'
'Bian, Yixuan'
'Lin, Zhien'
'Huang, Hui'
_publ_section_title
;
 Solvent-free synthesis of new metal phosphate-oxalates: influence of
 different metal ions on the framework structures.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13485
_journal_page_last               13489
_journal_paper_doi               10.1039/c5dt01613d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C H3 In O10 P2, C2 H7 N'
_chemical_formula_sum            'C3 H10 In N O10 P2'
_chemical_formula_weight         396.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_date             2015-06-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-06-11 deposited with the CCDC.
2015-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                91.768(5)
_cell_angle_beta                 111.205(6)
_cell_angle_gamma                115.495(6)
_cell_formula_units_Z            2
_cell_length_a                   7.6595(6)
_cell_length_b                   8.4550(4)
_cell_length_c                   9.6469(6)
_cell_measurement_reflns_used    3941
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.0340
_cell_measurement_theta_min      3.9440
_cell_volume                     512.65(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   -1.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.5694   57.0000   90.0000 84

  2 omega   -1.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.5694   57.0000 -180.0000 84

  3 omega  -11.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.5694   77.0000  -90.0000 94

  4 omega  -52.00   32.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.5694  -57.0000 -180.0000 84

  5 omega   -1.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.5694   57.0000    0.0000 84

  6 omega   35.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.5694  178.0000    0.0000 53

  7 omega   35.00   72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.5694  178.0000 -180.0000 37

  8 omega  -20.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.5694  -99.0000   30.0000 75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0443074000
_diffrn_orient_matrix_UB_12      0.0281177000
_diffrn_orient_matrix_UB_13      -0.0663521000
_diffrn_orient_matrix_UB_21      0.0679969000
_diffrn_orient_matrix_UB_22      0.0910515000
_diffrn_orient_matrix_UB_23      0.0397527000
_diffrn_orient_matrix_UB_31      0.0783388000
_diffrn_orient_matrix_UB_32      0.0019084000
_diffrn_orient_matrix_UB_33      -0.0236302000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6283
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         3.398
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.667
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.571
_exptl_crystal_description       block
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0232
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0268P)²+0.3111P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1994
_reflns_number_total             2090
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt01613d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7035614--7035619.cif.'
_cod_original_cell_volume        512.64(6)
_cod_database_code               7035619
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
2.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
2.c Idealised tetrahedral OH refined as rotating group:
 O4(H4), O7(H7), O8(H8)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
In1 In 0.31418(3) 0.52882(3) 0.70205(2) 0.01314(9) Uani 1 1 d .
P1 P 0.20679(12) 0.76453(10) 0.43817(9) 0.01335(17) Uani 1 1 d .
P2 P 0.38903(14) 0.64715(11) 1.05605(9) 0.01832(18) Uani 1 1 d .
O1 O 0.2246(4) 0.7089(3) 0.5899(2) 0.0185(5) Uani 1 1 d .
O2 O 0.3867(3) 0.7792(3) 0.3983(2) 0.0177(5) Uani 1 1 d .
O3 O -0.0101(3) 0.6432(3) 0.3086(2) 0.0193(5) Uani 1 1 d .
O4 O 0.2195(4) 0.9567(3) 0.4588(3) 0.0196(5) Uani 1 1 d .
H4 H 0.3442 1.0339 0.5037 0.029 Uiso 1 1 calc GR
O5 O 0.4072(4) 0.6936(3) 0.9111(3) 0.0213(5) Uani 1 1 d .
O6 O 0.5800(4) 0.6404(3) 1.1701(3) 0.0212(5) Uani 1 1 d .
O7 O 0.3618(5) 0.7948(4) 1.1314(3) 0.0332(6) Uani 1 1 d .
H7 H 0.3687 0.7812 1.2167 0.050 Uiso 1 1 calc GR
O8 O 0.1866(4) 0.4619(3) 1.0207(3) 0.0347(6) Uani 1 1 d .
H8 H 0.1100 0.4321 0.9291 0.052 Uiso 1 1 calc GR
O9 O 0.6126(3) 0.6529(3) 0.6727(2) 0.0183(5) Uani 1 1 d .
O10 O 0.7536(3) 0.6398(3) 0.5106(3) 0.0192(5) Uani 1 1 d .
C1 C 0.6049(5) 0.5838(4) 0.5529(3) 0.0146(6) Uani 1 1 d .
C2 C 1.1087(6) 0.9215(5) 0.8772(4) 0.0226(7) Uani 1 1 d .
H2A H 1.2503 0.9596 0.9553 0.027 Uiso 1 1 calc R
H2B H 1.0246 0.7932 0.8652 0.027 Uiso 1 1 calc R
C3 C 1.0089(6) 1.0192(5) 0.9257(4) 0.0246(7) Uani 1 1 d .
H3A H 0.8684 0.9824 0.8465 0.030 Uiso 1 1 calc R
H3B H 1.0942 1.1475 0.9385 0.030 Uiso 1 1 calc R
N1 N 1.1217(5) 0.9595(4) 0.7303(3) 0.0234(6) Uani 1 1 d .
H1A H 0.9922 0.9279 0.6596 0.028 Uiso 1 1 calc GR
H1B H 1.1752 0.8969 0.7006 0.028 Uiso 1 1 calc GR
H1C H 1.2054 1.0763 0.7430 0.028 Uiso 1 1 calc GR
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'
In In -0.7276 1.3100 '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'
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 In1 O3 95.04(9) . 2_566
O1 In1 O5 88.39(9) . .
O1 In1 O6 176.14(8) . 2_667
O1 In1 O9 89.77(8) . .
O1 In1 O10 94.16(8) . 2_666
O3 In1 O6 86.71(9) 2_566 2_667
O3 In1 O9 166.11(8) 2_566 .
O3 In1 O10 91.27(8) 2_566 2_666
O5 In1 O3 92.97(9) . 2_566
O5 In1 O6 88.08(9) . 2_667
O5 In1 O9 100.20(9) . .
O5 In1 O10 174.85(8) . 2_666
O6 In1 O9 89.31(8) 2_667 .
O6 In1 O10 89.24(9) 2_667 2_666
O9 In1 O10 75.36(8) . 2_666
O1 P1 O4 105.98(12) . .
O2 P1 O1 112.39(12) . .
O2 P1 O3 111.68(13) . .
O2 P1 O4 108.84(12) . .
O3 P1 O1 112.18(13) . .
O3 P1 O4 105.30(13) . .
O5 P2 O6 114.36(14) . .
O5 P2 O7 107.27(13) . .
O5 P2 O8 110.56(14) . .
O6 P2 O7 107.70(15) . .
O6 P2 O8 108.65(14) . .
O7 P2 O8 108.08(16) . .
P1 O1 In1 135.43(13) . .
P1 O3 In1 134.30(13) . 2_566
P1 O4 H4 109.5 . .
P2 O5 In1 131.11(14) . .
P2 O6 In1 144.20(14) . 2_667
P2 O7 H7 109.5 . .
P2 O8 H8 109.5 . .
C1 O9 In1 115.06(19) . .
C1 O10 In1 114.55(18) . 2_666
O9 C1 O10 125.2(3) . .
O9 C1 C1 117.7(3) . 2_666
O10 C1 C1 117.0(3) . 2_666
H2A C2 H2B 108.1 . .
C3 C2 H2A 109.6 . .
C3 C2 H2B 109.6 . .
N1 C2 H2A 109.6 . .
N1 C2 H2B 109.6 . .
N1 C2 C3 110.3(3) . .
C2 C3 C3 111.4(4) . 2_777
C2 C3 H3A 109.4 . .
C2 C3 H3B 109.4 . .
C3 C3 H3A 109.4 2_777 .
C3 C3 H3B 109.4 2_777 .
H3A C3 H3B 108.0 . .
C2 N1 H1A 109.5 . .
C2 N1 H1B 109.5 . .
C2 N1 H1C 109.5 . .
H1A N1 H1B 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
In1 O1 2.103(2) .
In1 O3 2.110(2) 2_566
In1 O5 2.109(2) .
In1 O6 2.147(2) 2_667
In1 O9 2.197(2) .
In1 O10 2.219(2) 2_666
P1 O1 1.528(2) .
P1 O2 1.517(2) .
P1 O3 1.525(2) .
P1 O4 1.588(2) .
P2 O5 1.502(2) .
P2 O6 1.505(2) .
P2 O7 1.552(2) .
P2 O8 1.571(3) .
O3 In1 2.110(2) 2_566
O4 H4 0.8200 .
O6 In1 2.147(2) 2_667
O7 H7 0.8200 .
O8 H8 0.8200 .
O9 C1 1.249(4) .
O10 In1 2.219(2) 2_666
O10 C1 1.254(4) .
C1 C1 1.548(6) 2_666
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C2 C3 1.505(5) .
C2 N1 1.492(4) .
C3 C3 1.521(6) 2_777
C3 H3A 0.9700 .
C3 H3B 0.9700 .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
N1 H1C 0.8900 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 O2 0.82 1.83 2.644(3) 174.8 2_676
N1 H1A O10 0.89 2.32 2.917(4) 124.3 .
N1 H1B O1 0.89 2.12 2.996(3) 165.9 1_655
N1 H1C O6 0.89 2.15 3.024(4) 166.3 2_777
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
In1 O9 C1 O10 176.2(2) . .
In1 O9 C1 C1 -3.6(4) . 2_666
In1 O10 C1 O9 176.4(2) 2_666 .
In1 O10 C1 C1 -3.9(4) 2_666 2_666
O1 P1 O3 In1 21.9(2) . 2_566
O2 P1 O1 In1 -39.1(2) . .
O2 P1 O3 In1 149.10(17) . 2_566
O3 P1 O1 In1 87.8(2) . .
O4 P1 O1 In1 -157.84(17) . .
O4 P1 O3 In1 -92.93(19) . 2_566
O5 P2 O6 In1 -120.6(2) . 2_667
O6 P2 O5 In1 91.8(2) . .
O7 P2 O5 In1 -148.86(19) . .
O7 P2 O6 In1 120.3(2) . 2_667
O8 P2 O5 In1 -31.2(2) . .
O8 P2 O6 In1 3.5(3) . 2_667
N1 C2 C3 C3 179.2(4) . 2_777
