#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/59/2015993.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2015993
loop_
_publ_author_name
'Cong Deng'
'Bi-Zhou Lin'
'Guo-Hua Han'
'Ling Bai'
_publ_section_title
;
 Poly[propane-1,3-diammonium [tetra-μ₃-oxo-hexaoxotrimolybdenum(VI)]
 dihydrate]
;
_journal_coeditor_code           GZ3086
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m256
_journal_page_last               m258
_journal_paper_doi               10.1107/S0108270107021051
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C3 H12 N2) [Mo3 O10], 2H2 O'
_chemical_formula_moiety         'C3 H12 N2 2+, Mo3 O10 2-, 2(H2 O)'
_chemical_formula_sum            'C3 H16 Mo3 N2 O12'
_chemical_formula_weight         560.00
_chemical_name_systematic
;
Poly[propylene-1,3-diammonium [tetra-μ₃-oxo-hexaoxotrimolybdenum(VI)]
dihydrate]
;
_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-97
_cell_angle_alpha                107.86(2)
_cell_angle_beta                 96.556(7)
_cell_angle_gamma                94.816(6)
_cell_formula_units_Z            2
_cell_length_a                   7.6330(15)
_cell_length_b                   8.7000(17)
_cell_length_c                   11.174(2)
_cell_measurement_reflns_used    3714
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      28.14
_cell_measurement_theta_min      2.47
_cell_volume                     696.1(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  SHELX97
_computing_structure_refinement  'SHELX97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELX97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
;
Bruker SMART APEXII CCD area-detector
;
_diffrn_measurement_method       'φ and ω'
_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  0.0028
_diffrn_reflns_av_sigmaI/netI    0.0103
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5476
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.722
_exptl_absorpt_correction_T_max  0.8759
_exptl_absorpt_correction_T_min  0.6400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.947
_refine_ls_extinction_coef       0.0052(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         2738
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1105P)²+1.8518P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1362
_reflns_number_gt                2699
_reflns_number_total             2738
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gz3086.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2015993
_cod_database_fobs_code          2015993
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Mo Mo1 0.21194(2) 0.26019(2) 0.408198(17) 0.02240(5) Uani d D 1
Mo Mo2 0.47932(3) 0.53795(2) 0.349695(18) 0.02256(5) Uani d D 1
Mo Mo3 0.02163(3) 0.46293(2) 0.650745(18) 0.02255(5) Uani d D 1
O O1 0.2157(3) 0.1099(2) 0.47459(17) 0.0368(5) Uani d D 1
O O2 0.1755(3) 0.1651(3) 0.24814(16) 0.0373(6) Uani d D 1
O O3 -0.0089(3) 0.3325(3) 0.4408(2) 0.0375(6) Uani d . 1
O O4 0.4646(3) 0.3312(3) 0.44328(19) 0.0358(5) Uani d . 1
O O5 0.2268(3) 0.5036(3) 0.37050(19) 0.0357(5) Uani d . 1
O O6 0.2614(3) 0.4321(3) 0.60831(19) 0.0366(5) Uani d . 1
O O7 0.4771(3) 0.4019(2) 0.20316(17) 0.0356(5) Uani d D 1
O O8 0.4524(3) 0.7158(2) 0.32085(19) 0.0388(6) Uani d D 1
O O9 -0.0302(3) 0.2863(2) 0.68011(19) 0.0365(5) Uani d D 1
O O10 0.0929(3) 0.5987(3) 0.79770(18) 0.0415(6) Uani d D 1
O O11 0.1810(3) 0.8224(3) 0.1375(2) 0.0439(6) Uani d D 1
H H11A 0.184(5) 0.796(2) 0.2132(17) 0.053 Uiso d D 1
H H11B 0.219(5) 0.933(2) 0.160(3) 0.053 Uiso d D 1
O O12 0.6788(4) 0.4708(4) 0.0017(3) 0.0607(8) Uani d D 1
H H12A 0.657(5) 0.454(4) 0.0785(16) 0.073 Uiso d D 1
H H12B 0.696(5) 0.370(3) -0.050(2) 0.073 Uiso d D 1
N N1 0.1518(4) 0.2381(4) 1.0154(3) 0.0557(9) Uani d . 1
H H1C 0.1667 0.2536 1.0986 0.067 Uiso calc R 1
H H1D 0.0377 0.2054 0.9834 0.067 Uiso calc R 1
H H1E 0.1857 0.3310 1.0017 0.067 Uiso calc R 1
N N2 0.3087(4) -0.1123(4) 0.6079(3) 0.0479(8) Uani d . 1
H H2C 0.3798 -0.1860 0.5766 0.057 Uiso calc R 1
H H2D 0.3236 -0.0306 0.5763 0.057 Uiso calc R 1
H H2E 0.1961 -0.1581 0.5864 0.057 Uiso calc R 1
C C1 0.2590(5) 0.1142(4) 0.9538(3) 0.0480(9) Uani d . 1
H H1A 0.2255 0.0158 0.9738 0.058 Uiso calc R 1
H H1B 0.3828 0.1513 0.9897 0.058 Uiso calc R 1
C C2 0.2418(5) 0.0719(5) 0.8094(3) 0.0479(10) Uani d . 1
H H2A 0.1186 0.0316 0.7733 0.057 Uiso calc R 1
H H2B 0.2719 0.1708 0.7893 0.057 Uiso calc R 1
C C3 0.3532(5) -0.0489(5) 0.7488(3) 0.0471(9) Uani d . 1
H H3A 0.3410 -0.1394 0.7821 0.056 Uiso calc R 1
H H3B 0.4765 -0.0004 0.7712 0.056 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'
Mo Mo -1.6832 0.6857 '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'
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
O1 Mo1 O2 . . 105.74(10)
O1 Mo1 O3 . . 101.65(11)
O2 Mo1 O3 . . 102.63(10)
O1 Mo1 O4 . . 97.02(10)
O2 Mo1 O4 . . 103.27(10)
O3 Mo1 O4 . . 142.39(9)
O1 Mo1 O6 . . 85.93(9)
O2 Mo1 O6 . . 168.33(10)
O3 Mo1 O6 . . 74.54(8)
O4 Mo1 O6 . . 74.57(8)
O1 Mo1 O5 . . 165.53(8)
O2 Mo1 O5 . . 88.66(9)
O3 Mo1 O5 . . 75.98(9)
O4 Mo1 O5 . . 77.85(9)
O6 Mo1 O5 . . 79.67(8)
O7 Mo2 O8 . . 103.99(10)
O7 Mo2 O6 . 2_666 94.16(9)
O8 Mo2 O6 . 2_666 99.01(10)
O7 Mo2 O5 . . 100.50(9)
O8 Mo2 O5 . . 91.74(10)
O6 Mo2 O5 2_666 . 159.19(10)
O7 Mo2 O4 . 2_666 163.26(10)
O8 Mo2 O4 . 2_666 90.36(9)
O6 Mo2 O4 2_666 2_666 74.81(8)
O5 Mo2 O4 . 2_666 87.43(8)
O7 Mo2 O4 . . 91.99(9)
O8 Mo2 O4 . . 161.23(9)
O6 Mo2 O4 2_666 . 89.42(9)
O5 Mo2 O4 . . 75.48(9)
O4 Mo2 O4 2_666 . 75.62(8)
O9 Mo3 O10 . . 103.55(11)
O9 Mo3 O5 . 2_566 91.58(10)
O10 Mo3 O5 . 2_566 100.35(10)
O9 Mo3 O6 . . 99.15(10)
O10 Mo3 O6 . . 94.75(10)
O5 Mo3 O6 2_566 . 158.91(10)
O9 Mo3 O3 . . 91.36(9)
O10 Mo3 O3 . . 162.26(10)
O5 Mo3 O3 2_566 . 88.61(8)
O6 Mo3 O3 . . 73.13(8)
O9 Mo3 O3 . 2_566 160.57(8)
O10 Mo3 O3 . 2_566 92.13(10)
O5 Mo3 O3 2_566 2_566 74.12(9)
O6 Mo3 O3 . 2_566 90.78(9)
O3 Mo3 O3 . 2_566 75.50(9)
Mo1 O3 Mo3 . . 106.29(9)
Mo1 O3 Mo3 . 2_566 102.92(10)
Mo3 O3 Mo3 . 2_566 104.50(9)
Mo1 O4 Mo2 . 2_666 105.24(10)
Mo1 O4 Mo2 . . 100.54(10)
Mo2 O4 Mo2 2_666 . 104.38(8)
Mo3 O5 Mo2 2_566 . 154.64(14)
Mo3 O5 Mo1 2_566 . 102.26(9)
Mo2 O5 Mo1 . . 101.40(9)
Mo2 O6 Mo3 2_666 . 152.95(11)
Mo2 O6 Mo1 2_666 . 103.29(9)
Mo3 O6 Mo1 . . 103.62(8)
H11A O11 H11B . . 107(2)
H12A O12 H12B . . 104(3)
C1 N1 H1C . . 109.5
C1 N1 H1D . . 109.5
H1C N1 H1D . . 109.5
C1 N1 H1E . . 109.5
H1C N1 H1E . . 109.5
H1D N1 H1E . . 109.5
C3 N2 H2C . . 109.5
C3 N2 H2D . . 109.5
H2C N2 H2D . . 109.5
C3 N2 H2E . . 109.5
H2C N2 H2E . . 109.5
H2D N2 H2E . . 109.5
N1 C1 C2 . . 115.0(3)
N1 C1 H1A . . 108.5
C2 C1 H1A . . 108.5
N1 C1 H1B . . 108.5
C2 C1 H1B . . 108.5
H1A C1 H1B . . 107.5
C3 C2 C1 . . 114.7(3)
C3 C2 H2A . . 108.6
C1 C2 H2A . . 108.6
C3 C2 H2B . . 108.6
C1 C2 H2B . . 108.6
H2A C2 H2B . . 107.6
C2 C3 N2 . . 113.6(3)
C2 C3 H3A . . 108.8
N2 C3 H3A . . 108.8
C2 C3 H3B . . 108.8
N2 C3 H3B . . 108.8
H3A C3 H3B . . 107.7
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
Mo1 O1 . 1.690(2) yes
Mo1 O2 . 1.7032(17) yes
Mo1 O3 . 1.884(2) yes
Mo1 O4 . 1.932(2) yes
Mo1 O6 . 2.245(2) yes
Mo1 O5 . 2.278(2) yes
Mo2 O7 . 1.6980(17) yes
Mo2 O8 . 1.699(2) yes
Mo2 O6 2_666 1.957(2) yes
Mo2 O5 . 1.976(2) yes
Mo2 O4 2_666 2.215(2) yes
Mo2 O4 . 2.342(2) yes
Mo3 O9 . 1.6923(19) yes
Mo3 O10 . 1.6989(18) yes
Mo3 O5 2_566 1.942(2) yes
Mo3 O6 . 1.962(2) yes
Mo3 O3 . 2.246(2) yes
Mo3 O3 2_566 2.312(3) yes
O3 Mo3 2_566 2.312(3) ?
O4 Mo2 2_666 2.215(2) ?
O5 Mo3 2_566 1.942(2) ?
O6 Mo2 2_666 1.957(2) ?
O11 H11A . 0.939(19) ?
O11 H11B . 0.927(17) ?
O12 H12A . 0.94(2) ?
O12 H12B . 0.92(2) ?
N1 C1 . 1.458(5) ?
N1 H1C . 0.8900 ?
N1 H1D . 0.8900 ?
N1 H1E . 0.8900 ?
N2 C3 . 1.488(4) ?
N2 H2C . 0.8900 ?
N2 H2D . 0.8900 ?
N2 H2E . 0.8900 ?
C1 C2 . 1.529(5) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C2 C3 . 1.460(5) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 H3A . 0.9700 ?
C3 H3B . 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
_geom_hbond_publ_flag
O11 H11A O8 . 0.939(19) 2.52(3) 3.142(3) 124(3) yes
O11 H11A O9 2_566 0.939(19) 2.00(3) 2.812(3) 143(3) yes
O11 H11B O2 1_565 0.927(17) 2.03(2) 2.861(3) 148(3) yes
O12 H12A O7 . 0.94(2) 2.18(3) 3.044(4) 152(3) yes
O12 H12A O10 2_666 0.94(2) 2.39(3) 2.923(4) 116(3) ?
O12 H12B O11 2_665 0.92(2) 2.03(3) 2.911(4) 161(3) yes
N1 H1C O2 1_556 0.89 2.04 2.851(4) 150.9 yes
N1 H1D O11 2_566 0.89 1.97 2.807(4) 155.9 yes
N1 H1E O12 2_666 0.89 1.95 2.815(5) 164.1 yes
N2 H2C O4 2_656 0.89 1.79 2.657(4) 164.9 yes
N2 H2D O1 . 0.89 2.07 2.866(4) 148.9 yes
N2 H2E O3 2_556 0.89 1.92 2.747(4) 153.6 yes
