# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_single_phase


_atom_sites_solution_secondary   iterative
#Added by publCIF




_atom_sites_solution_primary     direct
#Added by publCIF


_publcif_datablock.id            {4bae31b4-af1b-4180-b5e4-170c1e244509}

# 5. CHEMICAL DATA

_chemical_name_systematic        'bisnuth germanium oxyhydroxy nitrate'
_chemical_name_common            BiGeO2(OH)2(NO3)
# Get _chemical_formula_moiety using checkCIF
_chemical_formula_moiety         'Bi Ge N O7'
_chemical_formula_structural     'Bi Ge N O7'
_chemical_formula_analytical     'Bi Ge N O7'
_chemical_formula_sum            'Bi Ge N O7'
_chemical_formula_weight         408.631
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.0111 8.9310 'International Tables for Crystallography, Vol. C'
Ge Ge -1.0885 0.8855 'International Tables for Crystallography, Vol. C'
O O 0.0492 0.0322 'International Tables for Crystallography, Vol. C'
H H 0.0000 0.0000 'International Tables for Crystallography, Vol. C'
N N 0.0311 0.0180 'International Tables for Crystallography, Vol. C'

#===============================================================================
# 6. POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_Int_Tables_number      61

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x+1/2,-y,z+1/2
3 -x,y+1/2,-z+1/2
4 x+1/2,-y+1/2,-z
5 -x,-y,-z
6 x+1/2,y,-z+1/2
7 x,-y+1/2,z+1/2
8 -x+1/2,y+1/2,z

_cell_length_a                   11.4551(1)
_cell_length_b                   4.95346(5)
_cell_length_c                   18.1676(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1030.87(2)
# If checkCIF gives a different Z value, change both
# _chemical_formula_sum and _chemical_formula_weight.
_cell_formula_units_Z            8
_cell_measurement_temperature    303

_cell_special_details            orthorhombic

_exptl_crystal_density_diffrn    5.2647
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1432.00

# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to
# equatorial plane

_pd_spec_size_equat              ? # parallel to
# scattering vector
# in transmission

_pd_spec_size_thick              ? # parallel to
# scattering vector
# in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
'packed powder pellet'
_pd_spec_mount_mode              reflection

_pd_spec_shape                   flat_sheet

_pd_char_particle_morphology     thin_plate
_pd_char_colour                  white

# The following three fields describe the preparation of the specimen.
# The cooling rate is in K/min.  The pressure at which the sample was
# prepared is in kPa.  The temperature of preparation is in K.

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?

_exptl_absorpt_coefficient_mu    ?
# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_correction_type   ? # include if applicable
_exptl_absorpt_process_details   ? # include if applicable
_exptl_absorpt_correction_T_min  ? # include if applicable
_exptl_absorpt_correction_T_max  ? # include if applicable

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

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               ?
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
?

_diffrn_ambient_temperature      303
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              ?
_diffrn_measurement_device_type  'Rigaku SmartLab'
_diffrn_detector                 ?
_diffrn_detector_type            ?

_pd_meas_scan_method             step # options are 'step', 'cont',
#' 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         ?

loop_
_diffrn_radiation_type
_diffrn_radiation_wavelength
_diffrn_radiation_wavelength_wt
'Cu K\a~1~' 1.540593 1.0
#'Cu K\a~2~'  1.544427  0.333333
_diffrn_radiation_monochromator  No

# The following four items give details of the measured (not processed)
# powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        14501
_pd_meas_2theta_range_min        5.0000
_pd_meas_2theta_range_max        150.0000
_pd_meas_2theta_range_inc        0.0100

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/detc         ?
_pd_meas_2theta_fixed            ?

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

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      ?

# The next three items are given as text.

_pd_calc_method                  'Rietveld Refinement'

_pd_proc_ls_profile_function     'split pseudo-Voigt function'
_pd_proc_ls_background_function  'composite background function'
_pd_proc_ls_pref_orient_corr     no
# Replace '; ?' with the following four lines for the March-Dollase function:
#; $P_k = \sum_{j=1}^{m_k} \frac{1}{m_k}
#\left( r^2 \cos^2 \alpha_j +r^{-1}\ sin^2 \alpha_j \right)^{-3/2}$
#with a preferred-orientation vector, (hkl),
#and <i>r</i> = 1.0(0)

_pd_proc_ls_prof_R_factor        0.03465
_pd_proc_ls_prof_wR_factor       0.04654
_pd_proc_ls_prof_wR_expected     0.02347
_refine_ls_R_I_factor            0.01331
_refine_ls_R_Fsqd_factor         0.00768
_refine_ls_R_factor_all          0.00813

_refine_special_details          ?

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/yi
# The following line must be commented out in the absence of H atoms.
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     39
_refine_ls_number_restraints     0
_refine_ls_number_constraints    29

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   1.9828

_refine_ls_restrained_S_all      ?
# The following item can be obtained by setting NPRINT at 2 in *.ins.
_refine_ls_shift/su_max          0.0
_refine_ls_shift/su_mean         ?

_refine_diff_density_max         0.0
_refine_diff_density_min         0.0

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the
# intensities used in the refinement.

_pd_proc_2theta_range_min        5.0000
_pd_proc_2theta_range_max        150.0000
_pd_proc_2theta_range_inc        0.0100
_pd_proc_wavelength              ?


# Each refinement must be accompanied by a listing of the powder data
# in CIF format. Each listing should be sent as a separate file consisting
# of one data block containing a single powder profile. The value of
# _pd_block_diffractogram_id is used to associate each refinement with
# its corresponding powder profile, since it must match the value
# of _pd_block_id in the file containing the powder data. A template
# for supplying powder data in CIF format is available by ftp at
# ftp://ftp.iucr.org/pub/rietdataform.cif and an example is given
# at ftp://ftp.iucr.org/pub/rietdataxmpl.cif.

_pd_block_diffractogram_id       ?

# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

# The following items are used to identify the programs used.

_computing_data_collection       ?
_computing_cell_refinement       'RIETAN-FP (Izumi and Momma, 2007)'
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'RIETAN-FP (Izumi and Momma, 2007)'
_computing_molecular_graphics    'VESTA (Momma and Izumi, 2008)'
_computing_publication_material  ?

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

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_type_symbol
Bi1 0.39764(5) 0.3729(1) 0.18784(3) 1 8 c Uiso 0.00934(7) Bi
Ge1 0.3163(1) 0.5719(4) 0.8266(1) 1 8 c Uiso 0.0103(5) Ge
O1 0.2002(7) 0.102(3) 0.2890(5) 1 8 c Uiso 0.04433 O
O2 0.4458(8) 0.421(3) 0.7823(5) 1 8 c Uiso 0.04433 O
O3 0.3184(8) 0.568(2) 0.9208(5) 1 8 c Uiso 0.04433 Oh
N1 0.896(2) 0.586(3) 0.9096(7) 1 8 c Uiso 0.04433 N
O5 0.9707(8) 0.735(2) -0.0758(6) 1 8 c Uiso 0.04433 O
O6 0.6404(8) -0.078(2) 0.9566(5) 1 8 c Uiso 0.04433 O
O7 0.1489(7) 0.400(2) 0.1524(5) 1 8 c Uiso 0.04433 O
O4 0.5576(8) 0.269(2) 0.1243(5) 1 8 c Uiso 0.04433 O

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

#10. GEOMETRICAL PARAMETERS

_geom_special_details            ?

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Bi1 O2 2.134(9) . 5_666 ?
Bi1 O4 2.226(9) . 1_555 ?
Bi1 O2 2.32(1) . 7_554 ?
Bi1 O1 2.43(1) . 8_555 ?
Bi1 O7 2.48(1) . 8_545 ?
Bi1 O7 2.74(1) . 8_555 ?
Bi1 N1 2.88(1) . 4_456 ?
Bi1 O7 2.925(8) . 1_555 ?
Bi1 O5 2.93(1) . 4_465 ?
Bi1 O6 3.04(1) . 5_656 ?
Ge1 O3 1.712(9) . 1_555 ?
Ge1 O1 1.73(1) . 7_555 ?
Ge1 O1 1.76(1) . 2_565 ?
Ge1 O2 1.85(1) . 1_555 ?
Ge1 O4 1.873(9) . 5_666 ?
Ge1 Ge1 2.905(2) . 8_555 ?
Ge1 Ge1 2.905(2) . 8_545 ?
O1 Ge1 1.73(1) . 7_554 ?
O1 Ge1 1.76(1) . 2_564 ?
O1 O4 2.41(1) . 6_455 ?
O1 Bi1 2.43(1) . 8_545 ?
O1 O1 2.727(7) . 8_555 ?
O1 O1 2.727(7) . 8_545 ?
O1 O2 2.82(1) . 7_554 ?
O1 O3 2.88(1) . 7_554 ?
O1 O2 2.90(1) . 2_564 ?
O1 O3 2.91(1) . 2_564 ?
O1 O7 2.95(1) . 1_555 ?
O1 O2 3.09(1) . 2_554 ?
O2 Ge1 1.85(1) . 1_555 ?
O2 Bi1 2.134(9) . 5_666 ?
O2 O4 2.29(1) . 5_666 ?
O2 Bi1 2.32(1) . 7_555 ?
O2 O7 2.74(1) . 2_565 ?
O2 O1 2.82(1) . 7_555 ?
O2 O1 2.90(1) . 2_565 ?
O2 O5 2.90(2) . 8_646 ?
O2 O3 3.00(1) . 1_555 ?
O2 O2 3.01(1) . 3_646 ?
O2 O2 3.01(1) . 3_656 ?
O2 O7 3.06(2) . 4_556 ?
O2 O1 3.09(1) . 2_555 ?
O3 Ge1 1.712(9) . 1_555 ?
O3 O4 1.83(1) . 5_666 ?
O3 O1 2.88(1) . 7_555 ?
O3 O1 2.91(1) . 2_565 ?
O3 O5 2.93(1) . 8_646 ?
O3 O3 2.93(1) . 8_555 ?
O3 O3 2.93(1) . 8_545 ?
O3 O2 3.00(1) . 1_555 ?
N1 O5 1.17(2) . 1_556 ?
N1 O7 1.24(1) . 5_666 ?
N1 O6 1.25(2) . 8_655 ?
N1 O4 2.63(2) . 4_556 ?
N1 Bi1 2.88(1) . 4_556 ?
O5 N1 1.17(2) . 1_554 ?
O5 O7 2.07(1) . 5_665 ?
O5 O6 2.09(1) . 8_654 ?
O5 O4 2.79(1) . 4_565 ?
O5 O4 2.83(1) . 4_555 ?
O5 O2 2.90(2) . 8_654 ?
O5 O3 2.93(1) . 8_654 ?
O5 Bi1 2.93(1) . 4_565 ?
O5 O6 3.01(1) . 4_556 ?
O6 N1 1.25(2) . 8_645 ?
O6 O5 2.09(1) . 8_646 ?
O6 O7 2.17(1) . 4_556 ?
O6 O4 2.86(1) . 5_656 ?
O6 O5 3.01(1) . 4_456 ?
O6 Bi1 3.04(1) . 5_656 ?
O7 N1 1.24(1) . 5_666 ?
O7 O5 2.07(1) . 5_665 ?
O7 O6 2.17(1) . 4_456 ?
O7 Bi1 2.48(1) . 8_555 ?
O7 Bi1 2.74(1) . 8_545 ?
O7 O2 2.74(1) . 2_564 ?
O7 Bi1 2.925(8) . 1_555 ?
O7 O1 2.95(1) . 1_555 ?
O7 O4 3.03(1) . 8_555 ?
O7 O2 3.06(2) . 4_456 ?
O4 O3 1.83(1) . 5_666 ?
O4 Ge1 1.873(9) . 5_666 ?
O4 Bi1 2.226(9) . 1_555 ?
O4 O2 2.29(1) . 5_666 ?
O4 O1 2.41(1) . 6_555 ?
O4 N1 2.63(2) . 4_456 ?
O4 O5 2.79(1) . 4_465 ?
O4 O5 2.83(1) . 4_455 ?
O4 O6 2.86(1) . 5_656 ?
O4 O7 3.03(1) . 8_545 ?

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ge1 O1 113.6(5) 1_555 . 7_555 ?
O3 Ge1 O1 113.6(5) 1_555 . 2_565 ?
O3 Ge1 O2 114.8(4) 1_555 . 1_555 ?
O3 Ge1 O4 61.2(4) 1_555 . 5_666 ?
O1 Ge1 O1 102.8(4) 7_555 . 2_565 ?
O1 Ge1 O2 104.1(5) 7_555 . 1_555 ?
O1 Ge1 O4 173.5(5) 7_555 . 5_666 ?
O1 Ge1 O2 106.8(4) 2_565 . 1_555 ?
O1 Ge1 O4 83.2(4) 2_565 . 5_666 ?
O2 Ge1 O4 76.0(3) 1_555 . 5_666 ?
Ge1 O1 Ge1 112.8(5) 7_554 . 2_564 ?
Ge1 O3 O4 63.8(4) 1_555 . 5_666 ?
O5 N1 O7 118(2) 1_556 . 5_666 ?
O5 N1 O6 120(2) 1_556 . 8_655 ?
O7 N1 O6 121(2) 5_666 . 8_655 ?
O3 O4 Ge1 55.1(4) 5_666 . 5_666 ?

loop_
_publcif_info_exptl_table_extra_item
?

loop_
_publcif_info_exptl_table_header_item
?

_exptl_crystal_colour            white
_exptl_crystal_description       NA
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Heat-sensitive
_exptl_crystal_preparation       'precursor for synthesis of Bi4Ge3O12'
_database_code_depnum_ccdc_archive 'CCDC 1011413'
