Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Carole Morrison'
_publ_contact_author_address     
;
School of Chemistry
University of Edinburgh
The King's Buildings
West Mains Road
Edinburgh
Midlothian
EH9 3JJ
UNITED KINGDOM
;

_publ_contact_author_email       C.MORRISON@ED.AC.UK

_publ_section_title              
;
A New High Pressure Phase of Sodium Formate Dihydrate;
an Experimental and Computational Study
;
_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_creation_date             2006-09-05T14:11
_audit_author_name               'Bill Marshall'
_audit_update_record             
; 2006-09-05T14:11 Initial CIF as created by GSAS2CIF
;
_publ_requested_coeditor_name    D.R.Allan@ed.ac.uk
loop_
_publ_author_name
C.Morrison
D.Allan
W.G.Marshall
C.R.Pulham
M.Walker

# Attachment 'publish.cif'

data_CRYSTALS_cif
_database_code_depnum_ccdc_archive 'CCDC 627859'
_audit_creation_date             06-05-11
_audit_creation_method           CRYSTALS_ver_12.82

_oxford_structure_analysis_title 'naform in P 1 21 1'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   7.6852(9)
_cell_length_b                   3.5113(3)
_cell_length_c                   8.1103(17)
_cell_angle_alpha                90
_cell_angle_beta                 111.780(14)
_cell_angle_gamma                90
_cell_volume                     203.23(6)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'

_cell_formula_units_Z            2

# Given Formula = C1 H3 Na1 O3
# Dc = 1.41 Fooo = 108.00 Mu = 2.23 M = 86.02
# Found Formula = C1 H5 Na1 O4
# Dc = 1.70 FOOO = 108.00 Mu = 2.56 M = 104.04

_chemical_formula_sum            'C1 H5 Na1 O4'
_chemical_formula_moiety         'C1 H5 Na1 O4'
_chemical_compound_source        ?
_chemical_formula_weight         104.04

_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_max          0.10

_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_meas      ?
# Non-dispersive F(000):
_exptl_crystal_F_000             108
_exptl_absorpt_coefficient_mu    0.256

# Sheldrick geometric approximatio 0.97 0.97
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.9747
_exptl_absorpt_correction_T_max  0.9747
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       \w

_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  ?
_diffrn_standards_interval_count ?
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      293
_diffrn_reflns_number            369
_reflns_number_total             109
_diffrn_reflns_av_R_equivalents  0.035
# Number of reflections with Friedels Law is 109
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 264

_diffrn_reflns_theta_min         2.854
_diffrn_reflns_theta_max         22.455
_diffrn_measured_fraction_theta_max 0.344

_diffrn_reflns_theta_full        17.066
_diffrn_measured_fraction_theta_full 0.395

_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_reflns_limit_h_min              -8
_reflns_limit_h_max              4
_reflns_limit_k_min              0
_reflns_limit_k_max              3
_reflns_limit_l_min              0
_reflns_limit_l_max              6

_oxford_diffrn_Wilson_B_factor   1.45
_oxford_diffrn_Wilson_scale      0.27

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.24
_refine_diff_density_max         0.31

_refine_ls_number_reflns         104
_refine_ls_number_restraints     1
_refine_ls_number_parameters     25

#_refine_ls_R_factor_ref 0.0827
_refine_ls_wR_factor_ref         0.0893
_refine_ls_goodness_of_fit_ref   1.1988

#_reflns_number_all 107
_refine_ls_R_factor_all          0.0860
_refine_ls_wR_factor_all         0.0918

# The I/u(I) cutoff below was used for refinement as
# well as the _gt R-factors:
_reflns_threshold_expression     I>3.00u(I)
_reflns_number_gt                104
_refine_ls_R_factor_gt           0.0827
_refine_ls_wR_factor_gt          0.0893

_refine_ls_shift/su_max          0.002403

# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration unk

_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
2.35 -0.136 1.02
;

_publ_section_exptl_refinement   
;H atoms placed geometrically after each cycle
;

# Insert your own references if required - in alphabetical order
_publ_section_references         
;
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K., & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.

Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.

Siemens Industrial Automation, Inc (1993).
SMART: Area-Detector Software Package; Madison, WI.

Siemens Industrial Automation, Inc (1995).
SAINT: Area-Detector Integration Software.; Madison, WI.

Sheldrick, G.M. (1986). SHELXS86. Program for the solution of
crystal structures. Univ. of G\"ottingen, Federal Republic of Germany.

Watkin D.J. (1994).
Acta Cryst, A50, 411-437

Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, OXFORD, UK.
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Na1 Na 0.1830(16) 0.296(3) 0.642(3) 0.027(2) 1.0000 Uiso . . . . . .
C1 C 0.081(3) 0.317(6) 0.211(5) 0.015(4) 1.0000 Uiso . . . . . .
H1 H 0.0280 0.5008 0.1074 0.0500 1.0000 Uiso R . . . . .
O1 O 0.014(3) 0.291(4) 0.330(4) 0.021(3) 1.0000 Uiso . . . . . .
O2 O 0.241(3) 0.114(5) 0.246(6) 0.034(4) 1.0000 Uiso . . . . . .
O3 O 0.336(3) 0.318(5) 0.949(5) 0.055(4) 1.0000 Uiso . . . . . .
O4 O 0.376(3) 0.823(4) 0.605(5) 0.033(4) 1.0000 Uiso . . . . . .
H42 H 0.3366 0.9222 0.4946 0.0400 1.0000 Uiso R . . . . .
H41 H 0.4986 0.7645 0.6571 0.0400 1.0000 Uiso R . . . . .
H32 H 0.3015 0.2379 1.0372 0.0685 1.0000 Uiso R . . . . .
H31 H 0.4332 0.4809 0.9737 0.0685 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.18(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . H1 . 1.019 no
C1 . O1 . 1.25(3) yes
C1 . O2 . 1.36(3) yes
O3 . H32 . 0.900 no
O3 . H31 . 0.900 no
O4 . H42 . 0.900 no
O4 . H41 . 0.900 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
H1 . C1 . O1 . 121.8 no
H1 . C1 . O2 . 124.0 no
O1 . C1 . O2 . 114(3) yes
H32 . O3 . H31 . 119.0 no
H42 . O4 . H41 . 117.8 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O4 . H42 . O2 1_565 176.7 0.900 1.990 2.889 yes
O4 . H41 . O2 2_656 175.6 0.900 1.935 2.833 yes
O3 . H32 . O2 1_556 173.4 0.900 1.965 2.861 yes
O3 . H31 . O3 2_657 174.6 0.900 2.027 2.924 yes


# Information for phase 1
data_pd1
_database_code_depnum_ccdc_archive 'CCDC 634281'
_pd_block_id                     
2006-09-05T14:11|PRL48258_63_11TNS_PA_phase1|Bill_Marshall||

# Histograms for phase 1
loop_
_pd_block_diffractogram_id
2006-09-05T14:11|PRL48258_63_11TNS_PA_H_01|Bill_Marshall|PEARL-HiPr

#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products
_symmetry_space_group_name_Hall  ?

_exptl_crystal_F_000             ?
_exptl_crystal_density_diffrn    ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?

_cell_measurement_temperature    ?

_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

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

# 8. Phase information from GSAS

_pd_phase_name                   'Sodium formate dihydrate (P21)'
_cell_length_a                   7.6914(9)
_cell_length_b                   3.51868(27)
_cell_length_c                   8.1102(9)
_cell_angle_alpha                90.0
_cell_angle_beta                 111.806(8)
_cell_angle_gamma                90.0
_cell_volume                     203.786(23)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y+1/2,-z

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
Na Na 0.185(4) 0.296 0.6572(32) 1.0 Uani 0.00821 2
C C1 0.0931(17) 0.288(10) 0.2259(15) 1.0 Uani 0.00127 2
D D1 0.0248(28) 0.446(10) 0.1018(21) 1.0 Uani 0.03565 2
O O1 0.0168(20) 0.327(11) 0.3370(19) 1.0 Uani 0.01527 2
O O2 0.2457(20) 0.134(9) 0.2454(25) 1.0 Uani 0.01527 2
O O3 0.3522(27) 0.347(10) 0.9618(26) 1.0 Uani 0.0341 2
D D31 0.4217(31) 0.576(10) 0.0003(26) 1.0 Uani 0.04842 2
D D32 0.3033(29) 0.260(11) 0.0473(26) 1.0 Uani 0.04842 2
O O4 0.3618(27) 0.784(11) 0.5892(25) 1.0 Uani 0.0341 2
D D41 0.4945(26) 0.768(11) 0.6381(25) 1.0 Uani 0.04842 2
D D42 0.3414(29) 0.908(9) 0.4797(26) 1.0 Uani 0.04842 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_22
_atom_site_aniso_U_23
_atom_site_aniso_U_33
Na 0.008(5) 0.0 0.00305 0.00821 0.0 0.00821
C1 0.0013(26) 0.0 0.00047 0.00127 0.0 0.00127
D1 0.036(6) 0.0 0.01324 0.03565 0.0 0.03565
O1 0.0153(28) 0.0 0.00567 0.01527 0.0 0.01527
O2 0.0153(28) 0.0 0.00567 0.01527 0.0 0.01527
O3 0.034(4) 0.0 0.01266 0.0341 0.0 0.0341
D31 0.0484(34) 0.0 0.01799 0.04842 0.0 0.04842
D32 0.0484(34) 0.0 0.01799 0.04842 0.0 0.04842
O4 0.034(4) 0.0 0.01266 0.0341 0.0 0.0341
D41 0.0484(34) 0.0 0.01799 0.04842 0.0 0.04842
D42 0.0484(34) 0.0 0.01799 0.04842 0.0 0.04842

loop_
_atom_type_symbol
_atom_type_number_in_cell
Na 2.0
C 2.0
D 10.0
O 8.0

# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum            'C D5 Na O4'
_chemical_formula_weight         109.07
_cell_formula_units_Z            2

# MOLECULAR GEOMETRY

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
Na Na 3.51868(27) . 1_545 N
Na Na 3.51868(27) . 1_565 N
Na Na 3.51(5) . 2_546 N
Na Na 3.51(5) . 2_556 N
Na C1 3.190(27) . 2_546 N
Na C1 3.158(28) . 2_556 N
Na O1 2.436(30) . 1_555 N
Na O1 2.277(31) . 2_546 N
Na O1 2.440(34) . 2_556 N
Na O3 2.330(34) . 1_555 N
Na D31 2.874(32) . 1_556 N
Na D32 2.952(33) . 1_556 N
Na O4 2.440(34) . 1_545 N
Na O4 2.380(34) . 1_555 N
Na D41 3.068(33) . 1_545 N
Na D41 2.955(32) . 1_555 N
Na D42 2.583(27) . 1_545 N
Na D42 3.074(32) . 1_555 N
C1 Na 3.158(28) . 2_546 N
C1 Na 3.190(27) . 2_556 N
C1 D1 1.098(7) . 1_555 N
C1 O1 1.253(7) . 1_555 N
C1 O2 1.248(7) . 1_555 N
D1 C1 1.098(7) . 1_555 N
D1 O1 1.976(18) . 1_555 N
D1 O2 1.995(19) . 1_555 N
O1 Na 2.436(30) . 1_555 N
O1 Na 2.440(34) . 2_546 N
O1 Na 2.277(31) . 2_556 N
O1 C1 1.253(7) . 1_555 N
O1 D1 1.976(18) . 1_555 N
O2 C1 1.248(7) . 1_555 N
O2 D1 1.995(19) . 1_555 N
O2 D32 1.873(23) . 1_555 N
O2 D41 1.926(22) . 2_646 N
O2 D42 1.934(26) . 1_545 N
O3 Na 2.330(34) . 1_555 N
O3 D31 0.951(7) . 1_556 N
O3 D31 1.907(25) . 2_646 N
O3 D32 0.954(7) . 1_556 N
D31 Na 2.874(32) . 1_554 N
D31 O3 0.951(7) . 1_554 N
D31 O3 1.907(25) . 2_656 N
D31 D32 1.570(24) . 1_555 N
D32 Na 2.952(33) . 1_554 N
D32 O2 1.873(23) . 1_555 N
D32 O3 0.954(7) . 1_554 N
D32 D31 1.570(24) . 1_555 N
O4 Na 2.380(34) . 1_555 N
O4 Na 2.440(34) . 1_565 N
O4 D41 0.949(7) . 1_555 N
O4 D42 0.949(7) . 1_555 N
D41 Na 2.955(32) . 1_555 N
D41 Na 3.068(33) . 1_565 N
D41 O2 1.926(22) . 2_656 N
D41 O4 0.949(7) . 1_555 N
D41 D42 1.468(29) . 1_555 N
D42 Na 3.074(32) . 1_555 N
D42 Na 2.583(27) . 1_565 N
D42 O2 1.934(26) . 1_565 N
D42 O4 0.949(7) . 1_555 N
D42 D41 1.468(29) . 1_555 N

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
Na Na Na 180.0 1_545 . 1_565 N
Na Na Na 59.9(4) 1_545 . 2_546 N
Na Na Na 120.1(4) 1_545 . 2_556 N
Na Na O1 92.6(9) 1_545 . 1_555 N
Na Na O1 43.6(8) 1_545 . 2_546 N
Na Na O1 140.0(7) 1_545 . 2_556 N
Na Na O3 94.4(9) 1_545 . 1_555 N
Na Na O4 42.4(8) 1_545 . 1_545 N
Na Na O4 136.2(8) 1_545 . 1_555 N
Na Na D42 58.1(7) 1_545 . 1_545 N
Na Na Na 120.1(4) 1_565 . 2_546 N
Na Na Na 59.9(4) 1_565 . 2_556 N
Na Na O1 87.4(9) 1_565 . 1_555 N
Na Na O1 136.4(8) 1_565 . 2_546 N
Na Na O1 40.0(7) 1_565 . 2_556 N
Na Na O3 85.6(9) 1_565 . 1_555 N
Na Na O4 137.6(8) 1_565 . 1_545 N
Na Na O4 43.8(8) 1_565 . 1_555 N
Na Na D42 121.9(7) 1_565 . 1_545 N
Na Na Na 60.2(9) 2_546 . 2_556 N
Na Na O1 44.1(10) 2_546 . 1_555 N
Na Na O1 43.7(5) 2_546 . 2_546 N
Na Na O1 92.8(11) 2_546 . 2_556 N
Na Na O3 142.1(11) 2_546 . 1_555 N
Na Na O4 80.5(8) 2_546 . 1_545 N
Na Na O4 124.9(12) 2_546 . 1_555 N
Na Na D42 75.5(8) 2_546 . 1_545 N
Na Na O1 40.2(8) 2_556 . 1_555 N
Na Na O1 90.2(11) 2_556 . 2_546 N
Na Na O1 44.0(4) 2_556 . 2_556 N
Na Na O3 135.3(10) 2_556 . 1_555 N
Na Na O4 125.1(11) 2_556 . 1_545 N
Na Na O4 81.3(7) 2_556 . 1_555 N
Na Na D42 106.2(10) 2_556 . 1_545 N
O1 Na O1 87.6(11) 1_555 . 2_546 N
O1 Na O1 84.1(9) 1_555 . 2_556 N
O1 Na O3 172.8(16) 1_555 . 1_555 N
O1 Na O4 84.9(10) 1_555 . 1_545 N
O1 Na O4 81.0(9) 1_555 . 1_555 N
O1 Na D42 66.6(8) 1_555 . 1_545 N
O1 Na O1 96.4(9) 2_546 . 2_556 N
O1 Na O3 98.4(11) 2_546 . 1_555 N
O1 Na O4 84.9(13) 2_546 . 1_545 N
O1 Na O4 168.6(13) 2_546 . 1_555 N
O1 Na D42 95.2(12) 2_546 . 1_545 N
O1 Na O3 91.4(10) 2_556 . 1_555 N
O1 Na O4 168.9(12) 2_556 . 1_545 N
O1 Na O4 82.8(11) 2_556 . 1_555 N
O1 Na D42 147.8(11) 2_556 . 1_545 N
O3 Na O4 99.3(12) 1_555 . 1_545 N
O3 Na O4 93.0(12) 1_555 . 1_555 N
O3 Na D42 116.3(13) 1_555 . 1_545 N
O4 Na O4 93.8(10) 1_545 . 1_555 N
O4 Na D42 21.54(28) 1_545 . 1_545 N
O4 Na D42 80.1(10) 1_555 . 1_545 N
D1 C1 O1 114.3(16) 1_555 . 1_555 N
D1 C1 O2 116.3(17) 1_555 . 1_555 N
O1 C1 O2 128.8(16) 1_555 . 1_555 N
Na O1 Na 92.0(12) 1_555 . 2_546 N
Na O1 Na 96.1(10) 1_555 . 2_556 N
Na O1 C1 123.9(12) 1_555 . 1_555 N
Na O1 Na 96.4(9) 2_546 . 2_556 N
Na O1 C1 113.6(15) 2_546 . 1_555 N
Na O1 C1 126.8(16) 2_556 . 1_555 N
Na O3 D31 115.8(21) 1_555 . 1_556 N
Na O3 D32 122.3(19) 1_555 . 1_556 N
D31 O3 D32 110.9(25) 1_556 . 1_556 N
Na O4 Na 93.8(10) 1_555 . 1_565 N
Na O4 D41 118.7(20) 1_555 . 1_555 N
Na O4 D42 129.7(23) 1_555 . 1_555 N
Na O4 D41 123.5(26) 1_565 . 1_555 N
Na O4 D42 87.7(17) 1_565 . 1_555 N
D41 O4 D42 101.3(28) 1_555 . 1_555 N
O4 D41 D42 39.3(14) 1_555 . 1_555 N
Na D42 O4 70.7(17) 1_565 . 1_555 N
Na D42 D41 94.4(14) 1_565 . 1_555 N
O4 D42 D41 39.4(14) 1_555 . 1_555 N

_refine_ls_shift/su_max          0.02
_refine_ls_shift/su_mean         0.01
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     73
_refine_ls_goodness_of_fit_all   1.10
_refine_ls_number_restraints     7
_refine_ls_matrix_type           full