# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012

#Added by publCIF

data_New_Global_Publ_Block
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
#TrackingRef '- GePO-1 (CSD-424507)-revised.cif'

_publ_section_related_literature ?

# Added by publCIF - use a unique identifier for each data block

#==============================================================================

# SUBMISSION DETAILS

_publ_contact_author_name        'Lei Liu' # Name of author for correspondence
_publ_contact_author_address     # Address of author for correspondence
;
Research Institute of Special Chemicals, Taiyuan University of Technology,
Taiyuan030024,China.
;

_publ_contact_author_email       liulei@tyut.edu.cn
_publ_contact_author_fax         86-351-6111178
_publ_contact_author_phone       86-3516010550-5

_publ_contact_letter             
;
Please consider this CIF for publication. I certify that this contibution is the
original work of those listed as authors; that it has not been published
before (in any language or medium) and is not being considered for publication
elsewhere; that all authors concur with and are aware of the submission; that
all workers involved in the study are listed as authors or given proper credit
in the acknowledgements; that I have obtained permission for and acknowledged
the source of any excerpts from other copyright works; and that to the best of
my knowledge the paper contains no statements which are libellous, unlawful or
in any way actionable. All coauthors have made significant scientific
contributions to the work reported, including the ideas and their execution,
and share responsibility and accountability for the results.
;
_publ_requested_category         ?

#==============================================================================

# TITLE AND AUTHOR LIST

_publ_section_title              
;
The first ionothermal synthesis of a germanium phosphate with one-dimensional
chain structure
;
_publ_section_title_footnote     # remove if not required
.

# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary.

# NB if using publCIF, the Author database tool might prove useful
# (see the Tools menu in publCIF)

loop_
_publ_author_name
_publ_author_address
_publ_author_footnote
'Wei Wang'
;
Research Institute of Special Chemicals, Taiyuan University of Technology,
Taiyuan030024,China.
;
.
'Yang Li'
;
University of St Andrews,Purdie Building,St Andrews KY16 9ST, UK
;
.
'Lei Liu'
;
Research Institute of Special Chemicals, Taiyuan University of Technology,
Taiyuan030024,China.
;
.
'Jinxiang Dong'
;
Research Institute of Special Chemicals, Taiyuan University of Technology,
Taiyuan030024,China.
;
.

#==============================================================================

# TEXT

_publ_section_synopsis           .
_publ_section_abstract           
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(type here to add abstract)
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_publ_section_comment            
;
The stucture of the title compound, (I), is shown below. Dimensions are
available in the archived CIF.

For related literature, see [type here to add references to related
literature].
;
_publ_section_acknowledgements   # remove if not required
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(type here to add acknowledgements)
;
_publ_section_references         
;
?
;
_publ_section_figure_captions    
;

;
_publ_section_exptl_prep         
;
(type here to add preparation details)
;
_publ_section_exptl_refinement   
;
(type here to add refinement details)
;
#==============================================================================
_publ_manuscript_text            
# Used for convenience to store draft or replaced versions
# of the abstract, comment etc.
# Its contents will not be output
;
?
;

#==============================================================================

# Formatted by publCIF

data_GePO-1
_database_code_depnum_ccdc_archive 'CCDC 877718'
#TrackingRef '- GePO-1 (CSD-424507)-revised.cif'

_audit_update_record             
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2012-04-06 # Formatted by publCIF
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;

;
_chemical_name_common            TG27
_chemical_melting_point          ?
_chemical_formula_moiety         'Ge H6 N2 O8 P2, 2(H4 N), 0.38(H2 O)'
_chemical_formula_sum            'Ge H14.77 N4 O8.38 P2'
_chemical_formula_weight         340.8839

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ge Ge 0.1547 1.8001 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   10.644(4)
_cell_length_b                   5.1233(19)
_cell_length_c                   10.309(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.622(10)
_cell_angle_gamma                90.00
_cell_volume                     538.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    1135
_cell_measurement_theta_min      3.9957
_cell_measurement_theta_max      28.1382

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             344
_exptl_absorpt_coefficient_mu    3.179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7416
_exptl_absorpt_correction_T_max  0.9391
_exptl_absorpt_process_details   '(CrystalClear; Rigaku,2004)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  confocal
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 0.83
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            1869
_diffrn_reflns_av_R_equivalents  0.0123
_diffrn_reflns_av_sigmaI/netI    0.0132
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.00
_diffrn_reflns_theta_max         28.46
_reflns_number_total             627
_reflns_number_gt                615
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON(Spek,2003)
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
All the N-H bond distances were restrained to a 0.98\%A with a default
standard
deviation 0.03\%A in the refinement. The hydrogen atom of solvent water
molecule was not found on the solvent water molecule, and therefore, is not
included in the final structure. The isolated water molecule is strongly
disordered and partially occupied, and therefore, the O atom was refined
anisotropically and the occupancy of O atom was refined using a free variable.
The refinement was not able to determine definitely the isolated solvent
molecule was water rather than NH3 because the different assignments(O or N a
tom) of isolated molecule result in nearly the same R factor and the same size
of the ADP. However,the element analysis and the chemical possibility suggested
the isolated molecule was water molecule in the unit cell.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+1.2174P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         627
_refine_ls_number_parameters     66
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0176
_refine_ls_wR_factor_ref         0.0509
_refine_ls_wR_factor_gt          0.0503
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_restrained_S_all      1.156
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.5000 0.5000 0.0000 0.00404(13) Uani 1 4 d S . .
P1 P 0.54731(6) 1.0000 0.19512(6) 0.00381(16) Uani 1 2 d S . .
O3 O 0.63317(19) 1.0000 0.34063(18) 0.0101(4) Uani 1 2 d S . .
O2 O 0.40078(18) 1.0000 0.18125(18) 0.0068(4) Uani 1 2 d S . .
O1 O 0.58512(12) 0.7545(2) 0.12561(12) 0.0071(3) Uani 1 1 d . . .
N1 N 0.3442(2) 0.5000 0.0665(2) 0.0055(4) Uani 1 2 d SD . .
N2 N 0.7717(2) 0.5000 0.3779(2) 0.0095(5) Uani 1 2 d SD . .
O4 O 1.0000 1.0000 0.5000 0.116(12) Uani 0.38(2) 4 d SP . .
H5 H 0.831(3) 0.5000 0.320(3) 0.019(9) Uiso 1 2 d SD . .
H3 H 0.830(3) 0.5000 0.4705(15) 0.031(11) Uiso 1 2 d SD . .
H4 H 0.716(2) 0.656(3) 0.361(2) 0.020(6) Uiso 1 1 d D . .
H1 H 0.345(3) 0.342(3) 0.120(2) 0.025(7) Uiso 1 1 d D . .
H2 H 0.264(2) 0.5000 -0.009(2) 0.019(9) Uiso 1 2 d SD . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.0050(2) 0.00229(19) 0.0046(2) 0.000 0.00107(13) 0.000
P1 0.0058(3) 0.0025(3) 0.0027(3) 0.000 0.0006(2) 0.000
O3 0.0138(10) 0.0104(9) 0.0041(9) 0.000 -0.0007(7) 0.000
O2 0.0078(9) 0.0047(9) 0.0091(9) 0.000 0.0043(7) 0.000
O1 0.0060(6) 0.0052(6) 0.0094(6) -0.0041(5) 0.0010(5) -0.0003(5)
N1 0.0052(10) 0.0046(10) 0.0069(10) 0.000 0.0022(8) 0.000
N2 0.0113(11) 0.0111(12) 0.0057(11) 0.000 0.0017(8) 0.000
O4 0.081(14) 0.060(12) 0.25(3) 0.000 0.112(17) 0.000

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Ge1 O1 1.8778(13) 5_665 ?
Ge1 O1 1.8778(13) . ?
Ge1 O1 1.8778(13) 6_565 ?
Ge1 O1 1.8778(13) 2_655 ?
Ge1 N1 1.968(2) 5_665 ?
Ge1 N1 1.968(2) . ?
P1 O3 1.5169(19) . ?
P1 O2 1.525(2) . ?
P1 O1 1.5566(13) . ?
P1 O1 1.5566(13) 6_575 ?
N1 H1 0.978(3) . ?
N1 H2 0.979(3) . ?
N2 H5 0.979(3) . ?
N2 H3 0.979(3) . ?
N2 H4 0.979(3) . ?

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
O1 Ge1 O1 180.00(6) 5_665 . ?
O1 Ge1 O1 92.06(8) 5_665 6_565 ?
O1 Ge1 O1 87.94(8) . 6_565 ?
O1 Ge1 O1 87.94(8) 5_665 2_655 ?
O1 Ge1 O1 92.06(8) . 2_655 ?
O1 Ge1 O1 180.0 6_565 2_655 ?
O1 Ge1 N1 92.76(6) 5_665 5_665 ?
O1 Ge1 N1 87.24(6) . 5_665 ?
O1 Ge1 N1 87.24(6) 6_565 5_665 ?
O1 Ge1 N1 92.76(6) 2_655 5_665 ?
O1 Ge1 N1 87.24(6) 5_665 . ?
O1 Ge1 N1 92.76(6) . . ?
O1 Ge1 N1 92.76(6) 6_565 . ?
O1 Ge1 N1 87.24(6) 2_655 . ?
N1 Ge1 N1 180.00(10) 5_665 . ?
O3 P1 O2 113.79(11) . . ?
O3 P1 O1 107.05(7) . . ?
O2 P1 O1 110.43(6) . . ?
O3 P1 O1 107.05(7) . 6_575 ?
O2 P1 O1 110.43(6) . 6_575 ?
O1 P1 O1 107.83(10) . 6_575 ?
P1 O1 Ge1 137.84(8) . . ?
Ge1 N1 H1 108.8(15) . . ?
Ge1 N1 H2 111(2) . . ?
H1 N1 H2 108.4(18) . . ?
H5 N2 H3 105(3) . . ?
H5 N2 H4 110.5(17) . . ?
H3 N2 H4 111.1(18) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 P1 O1 Ge1 141.17(12) . . . . ?
O2 P1 O1 Ge1 16.80(15) . . . . ?
O1 P1 O1 Ge1 -103.94(12) 6_575 . . . ?
O1 Ge1 O1 P1 140(100) 5_665 . . . ?
O1 Ge1 O1 P1 -127.42(10) 6_565 . . . ?
O1 Ge1 O1 P1 52.58(10) 2_655 . . . ?
N1 Ge1 O1 P1 145.25(13) 5_665 . . . ?
N1 Ge1 O1 P1 -34.75(13) . . . . ?

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
N2 H5 O2 0.979(3) 1.796(10) 2.755(3) 166(3) 3_545
N2 H3 O3 0.979(3) 1.874(18) 2.786(3) 154(3) 7_666
N2 H4 O3 0.979(3) 1.957(6) 2.9259(17) 170(2) .
N2 H4 O1 0.979(3) 2.48(2) 3.075(2) 119.0(17) .
N1 H1 O2 0.978(3) 1.898(12) 2.8135(15) 155(2) 1_545
N1 H2 O2 0.979(3) 2.107(5) 3.084(3) 176(3) 7_565

_diffrn_measured_fraction_theta_max 0.830
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.078