# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Simon Parsons'
'Duncan J. Francis'
'Russell D L Johnstone'
'Alistair Lennie'
'William G Marshall'
'Stephen A Moggach'
'Elna Pidcock'
'John E Warren'

_publ_contact_author_name        'Simon Parsons'
_publ_contact_author_email       S.PARSONS@ED.AC.UK

_publ_section_title              
;
High-Pressure Polymorphism in L-Serine Monohydrate:
Identification of Driving Forces in High Pressure Phase Transitions and
Implications for Pressure-Induced Protein Denaturation
;

# Attachment 'all_structures.cif'

data_x_serhyI_10kbar
_database_code_depnum_ccdc_archive 'CCDC 692787'

#Serine hydrate I at 1 GPa.
#Pure single crystal Xray refinement.
#Edinburgh dataset code = serhy1

_oxford_structure_analysis_title 'serhy1 in P2(1)2(1)2(1)'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   9.3344(6)
_cell_length_b                   11.822(3)
_cell_length_c                   4.7387(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     522.92(14)

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

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 0.0010 0.0010 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'
N 0.0020 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0040 0.0030 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'

_cell_formula_units_Z            4

# Given Formula = C3 H9 N1 O4
# Dc = 1.56 Fooo = 264.00 Mu = 1.45 M = 123.11
# Found Formula = C3 H9 N1 O4
# Dc = 1.56 FOOO = 264.00 Mu = 1.45 M = 123.11

_chemical_formula_sum            'C3 H9 N1 O4'
_chemical_formula_moiety         'C3 H9 N1 O4'
_chemical_compound_source        ?
_chemical_formula_weight         123.11

_cell_measurement_reflns_used    604
_cell_measurement_theta_min      3
_cell_measurement_theta_max      16
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.10
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_max          0.20

_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_meas      ?
# Non-dispersive F(000):
_exptl_crystal_F_000             264
_exptl_absorpt_coefficient_mu    0.145

# Sheldrick geometric approximatio 0.97 0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.26
_exptl_absorpt_correction_T_max  0.99
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_type           ' synchrotron '
_diffrn_radiation_wavelength     0.48650
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_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_ambient_pressure         1000000
_diffrn_reflns_number            2795
_reflns_number_total             306
_diffrn_reflns_av_R_equivalents  0.0988
# Number of reflections with Friedels Law is 306
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 531
_diffrn_reflns_reduction_process 
;
Merged with SORTAV
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
;

_diffrn_reflns_theta_min         2.988
_diffrn_reflns_theta_max         17.662
_diffrn_measured_fraction_theta_max 0.473

_diffrn_reflns_theta_full        14.129
_diffrn_measured_fraction_theta_full 0.495

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       5
_reflns_limit_h_min              0
_reflns_limit_h_max              11
_reflns_limit_k_min              0
_reflns_limit_k_max              6
_reflns_limit_l_min              0
_reflns_limit_l_max              5

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

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

_refine_diff_density_min         -0.19
_refine_diff_density_max         0.18

_refine_ls_number_reflns         299
_refine_ls_number_restraints     85
_refine_ls_number_parameters     100

#_refine_ls_R_factor_ref 0.0531
_refine_ls_wR_factor_ref         0.0427
_refine_ls_goodness_of_fit_ref   1.0694

#_reflns_number_all 299
_refine_ls_R_factor_all          0.0531
_refine_ls_wR_factor_all         0.0427

# No actual I/u(I) cutoff was used for refinement. The
# threshold below is used for "_gt" information ONLY:
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                256
_refine_ls_R_factor_gt           0.0408
_refine_ls_wR_factor_gt          0.0411

_refine_ls_shift/su_max          0.000145

# 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 Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    refxyz # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     
;
Method=
SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6)
;

_publ_section_exptl_refinement   
;
Checkcif Output:

199_ALERT_1_A Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_A Check the Reported _diffrn_ambient_temperature . 293 K

Data were collected at 293K

022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.47
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 14.13 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.50
089_ALERT_3_A Poor Data / Parameter Ratio (Zmax .LT. 18) ..... 2.99
911_ALERT_3_B # Missing FCF Refl Between THmin & STh/l= 298
910_ALERT_3_C # Missing FCF Reflections Below TH(Min) ........ 3
912_ALERT_3_C # Missing FCF Reflections Above STH/L=0.6 ...... 40
340_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 5

The high pressure cell causes shading of a significant proportion of the
sphere of reflections. This means that the completeness is reduced.

042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?

The one given is chemically more meaningful

250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.14

This is probably due to the lack of information in one direction which occurs
as a result of the Merrill-Bassett diamond-anvil cell shading a significant
region of reciprocal space. The effect of this shading is often to cause a
smearing out of electron density in one particular direction.

731_ALERT_1_C Bond Calc 0.80(4), Rep 0.807(17) ...... 2.35 su-Rat
O3 -H7 1.555 1.555
731_ALERT_1_C Bond Calc 0.81(5), Rep 0.815(17) ...... 2.94 su-Rat
O4 -H8 1.555 1.555
731_ALERT_1_C Bond Calc 0.82(4), Rep 0.818(17) ...... 2.35 su-Rat
O4 -H9 1.555 1.555

This alert is due to the fact that PLATON calculates esds using only the
variances whereas CRYSTALS uses the full variance/covariance matrix.

;
# Insert your own references if required - in alphabetical order
_publ_section_references         
;
Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.

Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.

Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R.,
Munksgaard, Copenhagen, 291-294.

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

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

Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.

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
C1 C 0.5373(2) 0.2325(4) 0.3042(5) 0.0264 1.0000 Uani D U . . . .
C2 C 0.3998(3) 0.2490(4) 0.1372(5) 0.0303 1.0000 Uani D U . . . .
C3 C 0.3438(3) 0.3677(5) 0.1700(6) 0.0381 1.0000 Uani D U . . . .
N1 N 0.2920(2) 0.1642(5) 0.2190(5) 0.0333 1.0000 Uani D U . . . .
O1 O 0.54452(19) 0.1526(6) 0.4736(5) 0.0456 1.0000 Uani D U . . . .
O2 O 0.63545(16) 0.3031(4) 0.2597(4) 0.0310 1.0000 Uani D U . . . .
O3 O 0.32879(18) 0.3961(5) 0.4599(4) 0.0400 1.0000 Uani D U . . . .
O4 O 0.0795(2) -0.0044(5) 0.3484(5) 0.0385 1.0000 Uani D . . . . .
H1 H 0.4192(19) 0.237(2) -0.061(3) 0.0385 1.0000 Uiso D . . . . .
H2 H 0.413(2) 0.4188(19) 0.083(4) 0.0456 1.0000 Uiso D . . . . .
H3 H 0.2519(18) 0.374(2) 0.071(4) 0.0456 1.0000 Uiso D . . . . .
H4 H 0.266(2) 0.178(2) 0.393(4) 0.0517 1.0000 Uiso D . . . . .
H5 H 0.217(2) 0.170(3) 0.093(4) 0.0517 1.0000 Uiso D . . . . .
H6 H 0.335(2) 0.0967(17) 0.205(6) 0.0517 1.0000 Uiso D . . . . .
H7 H 0.260(4) 0.362(5) 0.515(8) 0.0607 1.0000 Uiso D . . . . .
H8 H 0.042(4) -0.039(6) 0.220(9) 0.0588 1.0000 Uiso D . . . . .
H9 H 0.007(3) 0.020(6) 0.424(8) 0.0588 1.0000 Uiso D . . . . .
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
C1 0.0215(11) 0.037(6) 0.0205(14) 0.000(3) 0.0049(10) -0.0022(17)
C2 0.0205(11) 0.052(6) 0.0186(11) 0.000(2) 0.0022(9) -0.0011(18)
C3 0.0263(13) 0.052(6) 0.0357(13) -0.006(3) -0.0015(12) 0.000(2)
N1 0.0207(10) 0.051(7) 0.0280(11) -0.002(2) -0.0008(9) -0.0028(19)
O1 0.0282(10) 0.058(7) 0.0511(15) 0.025(3) -0.0055(10) -0.0059(19)
O2 0.0247(8) 0.041(6) 0.0275(9) 0.0009(16) 0.0024(8) -0.0066(15)
O3 0.0280(10) 0.054(8) 0.0382(10) -0.009(2) 0.0078(8) -0.009(2)
O4 0.0389(12) 0.033(11) 0.0433(13) -0.007(2) -0.0056(9) 0.006(2)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.26(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 . C2 . 1.521(3) yes
C1 . O1 . 1.242(6) yes
C1 . O2 . 1.257(5) yes
C2 . C3 . 1.505(7) yes
C2 . N1 . 1.472(5) yes
C2 . H1 . 0.968(16) no
C3 . O3 . 1.422(4) yes
C3 . H2 . 0.976(16) no
C3 . H3 . 0.980(15) no
N1 . H4 . 0.874(16) no
N1 . H5 . 0.923(16) no
N1 . H6 . 0.894(17) no
O3 . H7 . 0.807(17) no
O4 . H8 . 0.815(17) no
O4 . H9 . 0.818(17) 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
C2 . C1 . O1 . 118.7(2) yes
C2 . C1 . O2 . 116.3(2) yes
O1 . C1 . O2 . 125.0(2) yes
C1 . C2 . C3 . 111.0(3) yes
C1 . C2 . N1 . 110.6(2) yes
C3 . C2 . N1 . 111.7(2) yes
C1 . C2 . H1 . 109.1(11) no
C3 . C2 . H1 . 107.8(14) no
N1 . C2 . H1 . 106.3(13) no
C2 . C3 . O3 . 110.8(3) yes
C2 . C3 . H2 . 107.8(13) no
O3 . C3 . H2 . 109.0(13) no
C2 . C3 . H3 . 109.1(15) no
O3 . C3 . H3 . 110.9(11) no
H2 . C3 . H3 . 109.2(14) no
C2 . N1 . H4 . 108.2(15) no
C2 . N1 . H5 . 107.5(14) no
H4 . N1 . H5 . 112.7(14) no
C2 . N1 . H6 . 106.5(13) no
H4 . N1 . H6 . 111.1(15) no
H5 . N1 . H6 . 110.6(15) no
C3 . O3 . H7 . 106(3) no
H8 . O4 . H9 . 99(4) no
_chemical_name_common            'Serine Monohydrate'
_exptl_crystal_recrystallization_method 'From H2O/EtOH'

data_x_serhyI_26kbar.cif
_database_code_depnum_ccdc_archive 'CCDC 692788'

#Serine hydrate I at 2.6 GPa.
#Pure single crystal Xray refinement.
#Edinburgh dataset code = serhy2

_oxford_structure_analysis_title 'serhy2 in P2(1)2(1)2(1)'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   9.3563(6)
_cell_length_b                   11.443(2)
_cell_length_c                   4.6166(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     494.28(10)

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

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 0.0010 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'
N 0.0020 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0040 0.0030 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'

_cell_formula_units_Z            4

# Given Formula = C3 H9 N1 O4
# Dc = 1.65 Fooo = 264.00 Mu = 1.54 M = 123.11
# Found Formula = C3 H9 N1 O4
# Dc = 1.65 FOOO = 264.00 Mu = 1.54 M = 123.11

_chemical_formula_sum            'C3 H9 N1 O4'
_chemical_formula_moiety         'C3 H9 N1 O4'
_chemical_compound_source        ?
_chemical_formula_weight         123.11

_cell_measurement_reflns_used    832
_cell_measurement_theta_min      3
_cell_measurement_theta_max      17
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.10
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_max          0.20

_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_meas      ?
# Non-dispersive F(000):
_exptl_crystal_F_000             264
_exptl_absorpt_coefficient_mu    0.154

# Sheldrick geometric approximatio 0.97 0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.34
_exptl_absorpt_correction_T_max  0.98
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_type           ' synchrotron '
_diffrn_radiation_wavelength     0.48650
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_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_ambient_pressure         2600000
_diffrn_reflns_number            2930
_reflns_number_total             311
_diffrn_reflns_av_R_equivalents  0.0898
# Number of reflections with Friedels Law is 311
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 506
_diffrn_reflns_reduction_process 
;
Merged with SORTAV
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
;

_diffrn_reflns_theta_min         1.925
_diffrn_reflns_theta_max         17.714
_diffrn_measured_fraction_theta_max 0.498

_diffrn_reflns_theta_full        13.463
_diffrn_measured_fraction_theta_full 0.535

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       5
_reflns_limit_h_min              0
_reflns_limit_h_max              11
_reflns_limit_k_min              0
_reflns_limit_k_max              6
_reflns_limit_l_min              0
_reflns_limit_l_max              5

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

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

_refine_diff_density_min         -0.19
_refine_diff_density_max         0.15

_refine_ls_number_reflns         307
_refine_ls_number_restraints     85
_refine_ls_number_parameters     100

#_refine_ls_R_factor_ref 0.0517
_refine_ls_wR_factor_ref         0.0497
_refine_ls_goodness_of_fit_ref   0.9923

#_reflns_number_all 307
_refine_ls_R_factor_all          0.0517
_refine_ls_wR_factor_all         0.0497

# No actual I/u(I) cutoff was used for refinement. The
# threshold below is used for "_gt" information ONLY:
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                264
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_gt          0.0478

_refine_ls_shift/su_max          0.000159

# 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 Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    refxyz # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     
;
Method=
SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6)
;

_publ_section_exptl_refinement   
;
Checkcif Output:

022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.50
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 13.46 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.54
089_ALERT_3_A Poor Data / Parameter Ratio (Zmax .LT. 18) ..... 3.07
911_ALERT_3_B # Missing FCF Refl Between THmin & STh/l= 271
912_ALERT_3_C # Missing FCF Reflections Above STH/L=0.6 ...... 43
340_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 5

The high pressure cell causes shading of a significant proportion of the
sphere of reflections. This means that the completeness is reduced.

199_ALERT_1_A Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_A Check the Reported _diffrn_ambient_temperature . 293 K

Data were collected at 293K

042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?

The one given is chemically more meaningful

250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.36

This is probably due to the lack of information in one direction which occurs
as a result of the Merrill-Bassett diamond-anvil cell shading a significant
region of reciprocal space. The effect of this shading is often to cause a
smearing out of electron density in one particular direction.

731_ALERT_1_C Bond Calc 0.82(5), Rep 0.825(17) ...... 2.94 su-Rat
O4 -H8 1.555 1.555
731_ALERT_1_C Bond Calc 0.83(4), Rep 0.828(17) ...... 2.35 su-Rat
O4 -H9 1.555 1.555

This alert is due to the fact that PLATON calculates esds using only the
variances whereas CRYSTALS uses the full variance/covariance matrix.

;
# Insert your own references if required - in alphabetical order
_publ_section_references         
;
Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.

Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.

Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R.,
Munksgaard, Copenhagen, 291-294.

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

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

Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.

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
C1 C 0.5405(2) 0.2349(4) 0.2945(5) 0.0269 1.0000 Uani D U . . . .
C2 C 0.3989(2) 0.2494(4) 0.1331(5) 0.0254 1.0000 Uani D U . . . .
C3 C 0.3404(2) 0.3697(5) 0.1741(5) 0.0289 1.0000 Uani D U . . . .
N1 N 0.29608(17) 0.1593(5) 0.2293(5) 0.0269 1.0000 Uani D U . . . .
O1 O 0.55313(17) 0.1505(5) 0.4624(5) 0.0456 1.0000 Uani D U . . . .
O2 O 0.63350(16) 0.3105(4) 0.2482(4) 0.0354 1.0000 Uani D U . . . .
O3 O 0.33047(16) 0.3969(4) 0.4730(4) 0.0318 1.0000 Uani D U . . . .
O4 O 0.07893(19) -0.0039(5) 0.3349(5) 0.0434 1.0000 Uani D . . . . .
H1 H 0.4171(18) 0.237(2) -0.074(3) 0.0303 1.0000 Uiso D . . . . .
H2 H 0.400(2) 0.4264(19) 0.082(4) 0.0340 1.0000 Uiso D . . . . .
H3 H 0.2475(17) 0.372(2) 0.086(4) 0.0340 1.0000 Uiso D . . . . .
H4 H 0.269(2) 0.172(2) 0.415(4) 0.0389 1.0000 Uiso D . . . . .
H5 H 0.2215(19) 0.162(2) 0.111(4) 0.0389 1.0000 Uiso D . . . . .
H6 H 0.337(2) 0.0899(17) 0.212(5) 0.0389 1.0000 Uiso D . . . . .
H7 H 0.247(2) 0.384(6) 0.516(6) 0.0444 1.0000 Uiso D . . . . .
H8 H 0.042(4) -0.040(7) 0.200(9) 0.0710 1.0000 Uiso D . . . . .
H9 H 0.009(3) 0.029(5) 0.409(8) 0.0710 1.0000 Uiso D . . . . .
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
C1 0.0175(9) 0.046(5) 0.0170(11) 0.000(2) 0.0031(8) 0.0007(14)
C2 0.0177(9) 0.041(5) 0.0181(10) 0.001(2) 0.0010(8) -0.0002(16)
C3 0.0214(10) 0.038(5) 0.0277(11) 0.003(2) -0.0001(9) -0.0022(19)
N1 0.0169(8) 0.037(6) 0.0274(11) -0.003(2) -0.0012(7) -0.0019(14)
O1 0.0255(7) 0.063(6) 0.0482(13) 0.023(2) -0.0061(8) -0.0027(17)
O2 0.0214(7) 0.059(6) 0.0263(9) 0.0026(17) 0.0034(7) -0.0078(13)
O3 0.0217(8) 0.040(6) 0.0339(9) -0.0059(17) 0.0072(7) -0.0027(16)
O4 0.0304(9) 0.063(9) 0.0370(12) -0.004(2) -0.0031(8) 0.0024(15)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.33(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 . C2 . 1.529(3) yes
C1 . O1 . 1.244(5) yes
C1 . O2 . 1.245(4) yes
C2 . C3 . 1.493(6) yes
C2 . N1 . 1.479(5) yes
C2 . H1 . 0.982(15) no
C3 . O3 . 1.417(3) yes
C3 . H2 . 0.955(17) no
C3 . H3 . 0.959(15) no
N1 . H4 . 0.904(16) no
N1 . H5 . 0.886(16) no
N1 . H6 . 0.885(17) no
O3 . H7 . 0.819(16) no
O4 . H8 . 0.825(17) no
O4 . H9 . 0.828(17) 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
C2 . C1 . O1 . 118.0(2) yes
C2 . C1 . O2 . 116.5(2) yes
O1 . C1 . O2 . 125.4(2) yes
C1 . C2 . C3 . 110.9(2) yes
C1 . C2 . N1 . 110.0(2) yes
C3 . C2 . N1 . 111.5(2) yes
C1 . C2 . H1 . 107.9(10) no
C3 . C2 . H1 . 109.0(13) no
N1 . C2 . H1 . 107.5(12) no
C2 . C3 . O3 . 110.5(3) yes
C2 . C3 . H2 . 110.8(13) no
O3 . C3 . H2 . 108.9(12) no
C2 . C3 . H3 . 108.0(14) no
O3 . C3 . H3 . 110.2(11) no
H2 . C3 . H3 . 108.5(14) no
C2 . N1 . H4 . 110.6(14) no
C2 . N1 . H5 . 107.7(14) no
H4 . N1 . H5 . 111.2(14) no
C2 . N1 . H6 . 108.4(13) no
H4 . N1 . H6 . 110.5(15) no
H5 . N1 . H6 . 108.3(15) no
C3 . O3 . H7 . 105(2) no
H8 . O4 . H9 . 102(4) no
_chemical_name_common            'Serine Monohydrate'
_exptl_crystal_recrystallization_method 'From H2O/EtOH'

data_x_serhyI_37kbar
_database_code_depnum_ccdc_archive 'CCDC 692789'

#Parameters quoted are from a joint X-N refinement of phase I

#Serine hydrate I at 3.7 GPa.
#X-N refinement. This cif contains data used to model the Xray data set.
#Edinburgh dataset code = serhy3

#Notes on this cif:
#The structural data comes from a joint X-N refinement (see text in paper)
#The majority of this cif was generated with CRYSTALS.
#The Topas cif was processed using Platon so that x's and u's conform to the
#'rule of 19'. The x's, u's and geometrical parameters were then pasted into
#this cif. R-factors: _refine_ls_wR_factor_ref corresponds to the Topas Rwp.
#Other R-factors were calculated by importing the final model into crystals
#and doing a structure factor calculation.

_oxford_structure_analysis_title 'serhy3 in P2(1)2(1)2(1)'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   9.3706(6)
_cell_length_b                   11.204(2)
_cell_length_c                   4.5341(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     476.02(10)

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

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 0.0010 0.0010 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'
N 0.0020 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0040 0.0030 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'

_cell_formula_units_Z            4

# Given Formula = C3 H9 N1 O4
# Dc = 1.72 Fooo = 264.00 Mu = 1.59 M = 123.11
# Found Formula = C3 H9 N1 O4
# Dc = 1.72 FOOO = 264.00 Mu = 1.59 M = 123.11

_chemical_formula_sum            'C3 H9 N1 O4'
_chemical_formula_moiety         'C3 H9 N1 O4'
_chemical_compound_source        ?
_chemical_formula_weight         123.11

_cell_measurement_reflns_used    597
_cell_measurement_theta_min      3
_cell_measurement_theta_max      17
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.10
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_max          0.20

_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_meas      ?
# Non-dispersive F(000):
_exptl_crystal_F_000             264
_exptl_absorpt_coefficient_mu    0.159

# Sheldrick geometric approximatio 0.97 0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.06
_exptl_absorpt_correction_T_max  0.98
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_type           ' Synchrotron '
_diffrn_radiation_wavelength     0.48650
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_structure_solution    'Frey et al'
_computing_structure_refinement  'Crystals and Topas'
_computing_publication_material  'Topas, Crystals and Platon'
_computing_molecular_graphics    Diamond

_diffrn_standards_interval_time  ?
_diffrn_standards_interval_count ?
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         3700000
_diffrn_reflns_number            2574
_reflns_number_total             288
_diffrn_reflns_av_R_equivalents  0.1235
# Number of reflections with Friedels Law is 288
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 495
_diffrn_reflns_reduction_process 
;
Merged with SORTAV
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
;

_diffrn_reflns_theta_min         2.976
_diffrn_reflns_theta_max         17.807
_diffrn_measured_fraction_theta_max 0.470

_diffrn_reflns_theta_full        13.890
_diffrn_measured_fraction_theta_full 0.481

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       5
_reflns_limit_h_min              0
_reflns_limit_h_max              11
_reflns_limit_k_min              0
_reflns_limit_k_max              6
_reflns_limit_l_min              0
_reflns_limit_l_max              5

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens   'from Frey et al'

_refine_diff_density_min         -0.19
_refine_diff_density_max         0.20

_refine_ls_number_reflns         275
_refine_ls_number_restraints     2
_refine_ls_number_parameters     131 #131 parameters in joint x-n refinement

_refine_ls_wR_factor_ref         0.07813
_refine_ls_goodness_of_fit_ref   1.559

#_reflns_number_all 275
_refine_ls_R_factor_all          0.0546
_refine_ls_wR_factor_all         0.0781

# No actual I/u(I) cutoff was used for refinement. The
# threshold below is used for "_gt" information ONLY:
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                233
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_gt          0.0947

_refine_ls_shift/su_max          0.000

# 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 syn

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    refall # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?

_publ_section_exptl_refinement   
;

Checkcif output:

022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.47
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 13.89 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.48
089_ALERT_3_A Poor Data / Parameter Ratio (Zmax .LT. 18) ..... 2.10

The high pressure cell causes shading of a significant proportion of the
sphere of reflections. This means that the completeness is reduced.

340_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 11

The Platon su calculation does not take the variance covarience off diagonal
terms into account. The C-C sus are actually much better than this: see text.

020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.12

Mostly due to weak data at high resolution.

042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
The one given is chemically more meaningful

125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?

No action

245_ALERT_2_C U(iso) H1 Smaller than U(eq) C2 by ... 0.02 AngSq
245_ALERT_2_C U(iso) H2 Smaller than U(eq) C3 by ... 0.02 AngSq
245_ALERT_2_C U(iso) H3 Smaller than U(eq) C3 by ... 0.02 AngSq
245_ALERT_2_C U(iso) H4 Smaller than U(eq) N1 by ... 0.02 AngSq
245_ALERT_2_C U(iso) H5 Smaller than U(eq) N1 by ... 0.02 AngSq
245_ALERT_2_C U(iso) H6 Smaller than U(eq) N1 by ... 0.02 AngSq
245_ALERT_2_C U(iso) H7 Smaller than U(eq) O3 by ... 0.03 AngSq
245_ALERT_2_C U(iso) H8 Smaller than U(eq) O4 by ... 0.03 AngSq
245_ALERT_2_C U(iso) H9 Smaller than U(eq) O4 by ... 0.03 AngSq

A common overall istropic parameter was refined for the H-atoms.
B(H, overall)= 0.44564 +- 0.29752

199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K

OK

791_ALERT_1_G Confirm the Absolute Configuration of C2 = . S
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 2

OK

;

# Insert your own references if required - in alphabetical order
_publ_section_references         
;
Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.

Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.

Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R.,
Munksgaard, Copenhagen, 291-294.

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

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

Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.

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_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
O1 O Uani 0.5579(7) 0.1506(8) 0.4547(18) 1.000 0.039(4) . .
O2 O Uani 0.6311(8) 0.3147(8) 0.2401(18) 1.000 0.024(3) . .
O3 O Uani 0.332(2) 0.396(2) 0.482(5) 1.000 0.032(3) . .
N1 N Uani 0.2990(9) 0.1544(10) 0.233(2) 1.000 0.025(4) . .
C1 C Uani 0.5409(2) 0.2368(3) 0.2882(5) 1.000 0.023(4) . .
C2 C Uani 0.3989(3) 0.2486(7) 0.1300(10) 1.000 0.022(4) . .
C3 C Uani 0.3379(11) 0.3727(15) 0.177(3) 1.000 0.025(5) . .
O4 O Uani 0.0786(2) -0.0017(6) 0.3261(6) 1.000 0.033(3) . .
H1 H Uiso 0.413(2) 0.2355(16) -0.075(4) 1.000 0.006(4) . .
H2 H Uiso 0.3977(19) 0.429(2) 0.083(5) 1.000 0.006(4) . .
H3 H Uiso 0.245(3) 0.376(2) 0.095(5) 1.000 0.006(4) . .
H4 H Uiso 0.2718(18) 0.1719(17) 0.412(4) 1.000 0.006(4) . .
H5 H Uiso 0.226(2) 0.1527(17) 0.115(4) 1.000 0.006(4) . .
H6 H Uiso 0.343(2) 0.0862(16) 0.231(4) 1.000 0.006(4) . .
H7 H Uiso 0.245(4) 0.383(3) 0.524(7) 1.000 0.006(4) . .
H8 H Uiso 0.041(2) -0.048(2) 0.197(4) 1.000 0.006(4) . .
H9 H Uiso 0.008(2) 0.0374(19) 0.399(4) 1.000 0.006(4) . .

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
O1 0.0224(10) 0.041(11) 0.0525(17) 0.025(3) -0.0061(10) -0.003(2)
O2 0.0223(9) 0.029(9) 0.0217(11) 0.0032(18) 0.0026(8) -0.0038(17)
O3 0.0194(10) 0.048(9) 0.0299(12) -0.006(2) 0.0043(8) -0.0021(19)
N1 0.0155(9) 0.034(11) 0.0242(13) -0.003(2) -0.0026(9) 0.001(2)
C1 0.0142(13) 0.038(12) 0.0158(14) 0.000(3) 0.0038(11) 0.002(2)
C2 0.0194(13) 0.028(13) 0.0185(14) 0.001(3) 0.0011(10) 0.000(3)
C3 0.0206(14) 0.031(14) 0.0230(15) -0.001(3) -0.0003(11) 0.004(3)
O4 0.0258(10) 0.042(10) 0.0314(12) -0.002(2) -0.0019(9) 0.0004(17)

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
O1 C1 1.236(9) . . yes
O2 C1 1.234(9) . . yes
O3 C3 1.41(3) . . yes
O3 H7 0.85(4) . . no
O4 H9 0.86(2) . . no
O4 H8 0.86(2) . . no
N1 C2 1.486(12) . . yes
N1 H5 0.87(2) . . no
N1 H4 0.87(2) . . no
N1 H6 0.87(2) . . no
C1 C2 1.517(4) . . no
C2 C3 1.518(18) . . no
C2 H1 0.950(19) . . no
C3 H3 0.95(3) . . no
C3 H2 0.95(3) . . no

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
C3 O3 H7 103(3) . . . no
H8 O4 H9 104.7(18) . . . no
C2 N1 H5 108.6(15) . . . no
C2 N1 H6 108.8(14) . . . no
H4 N1 H5 110.3(19) . . . no
H4 N1 H6 110(2) . . . no
H5 N1 H6 110(2) . . . no
C2 N1 H4 108.5(15) . . . no
O1 C1 O2 124.9(5) . . . yes
O2 C1 C2 117.1(5) . . . yes
O1 C1 C2 118.0(5) . . . yes
N1 C2 C1 110.0(5) . . . yes
N1 C2 C3 111.7(6) . . . yes
C1 C2 C3 110.1(6) . . . no
O3 C3 C2 108.8(13) . . . yes
N1 C2 H1 106.6(13) . . . no
C3 C2 H1 109.3(13) . . . no
C1 C2 H1 109.1(12) . . . no
O3 C3 H2 110(2) . . . no
O3 C3 H3 110.0(19) . . . no
C2 C3 H3 109.1(19) . . . no
H2 C3 H3 110(2) . . . no
C2 C3 H2 108.9(16) . . . no

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
O1 C1 C2 N1 5.1(8) . . . . no
O1 C1 C2 C3 128.6(8) . . . . no
O2 C1 C2 N1 -174.9(6) . . . . no
O2 C1 C2 C3 -51.4(8) . . . . no
N1 C2 C3 O3 68.6(12) . . . . no
C1 C2 C3 O3 -53.9(12) . . . . no

_chemical_name_common            'Serine Monohydrate'
_exptl_crystal_recrystallization_method 'From H2O/EtOH'

data_n_serhyI_38kbar.cif
_database_code_depnum_ccdc_archive 'CCDC 692790'

#X-N refinement of phase 1 at 3.8 GPa.

#Serine hydrate I at 3.8 GPa.
#X-N refinement. This cif contains strutural parameters used to
#model the neutron powder data set.
#ISIS data set code: PRL57149_54_40TNS_ASCII_TOF

_chemical_name_systematic        
;
perdeuterated L-serine hydrate
;
_chemical_name_common            'Serine hydrate'

_chemical_formula_moiety         'C3 D7 N O3, D2 O1'
_chemical_formula_structural     ?
_chemical_formula_sum            'C3 D9 N O4'
_chemical_formula_weight         132.13
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P212121
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_Int_Tables_number      19

_cell_length_a                   9.3701(14)
_cell_length_b                   11.1831(10)
_cell_length_c                   4.52938(59)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     474.62(10)

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

_cell_measurement_temperature    298
_cell_measurement_pressure       3805000 #3.805(12) GPa
_cell_measurement_reflns_used    1119
_cell_formula_units_Z            4

_cell_special_details            
;
Cell parameters included in refinement
;
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             ?

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_particle_morphology     Block
_pd_char_colour                  Colourless
_chemical_absolute_configuration rm

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS software.
;

_pd_instr_location               'ISIS, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      298
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            ?
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'HiPr/PEARL, ISIS'
_diffrn_radiation_monochromator  ?
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom
_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source

;

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_number            1119

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

_pd_instr_dist_src/spec          12600
_pd_instr_dist_spec/detc         600
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
Modelling of preferred orientation was found to be unnecessary.
;

_pd_proc_ls_prof_R_factor        1.956
_pd_proc_ls_prof_wR_factor       1.565
_pd_proc_ls_prof_R_expected      1.395
_refine_ls_goodness_of_fit_all   1.121

_refine_ls_matrix_type           sparse
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     131
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          <0.001

_pd_proc_info_excluded_regions   
;
excluded short TOF region above

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;

Refinement was carried out against neutron and X-ray data simultaneously.
The X-ray data had been collected using synchrotron radiation, and the
pressure (ruby fluorescence) was 3.7 GPa. wR2 = 7.813 and S = 1.559 for
pure 1/sigma^2 weights.

Checkcif output:

023_ALERT_3_A Resolution (too) Low [sin(th)/Lambda < 0.6]..... 0.00 Deg.
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 0.00 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.00
037_ALERT_1_A _diffrn_reflns_theta_full .......... Not Given . ?
038_ALERT_1_A _diffrn_measured_fraction_theta_max Not Given . ?
039_ALERT_1_A _diffrn_measured_fraction_theta_full Not Given . ?

The resolution range was 0.64 to 4.14 Ang.

050_ALERT_1_A Absorption Coefficient mu Missing .............. ?

TOF data - the absorption coefficient is variable.

095_ALERT_1_A No Residual Density Maximum Given .............. ?
096_ALERT_1_A No Residual Density Minimum Given .............. ?

These data are not yet output by TOPAS.

201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8
210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ?

Powder data: see text of paper.

340_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 11

This is quite good for a high pressure neutron powder refinement!

040_ALERT_1_C No H-atoms in this Carbon Containing Compound .. ?
720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 9

The sample was deuterated.

;

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
C1 C 0 0.54093(22) 0.23680(32) 0.28819(46) 1 0.802(84)
C2 C 0 0.39887(35) 0.24861(65) 0.13003(98) 1 0.802(84)
C3 C 0 0.3379(11) 0.3727(15) 0.1768(31) 1 0.802(84)
N1 N 0 0.29903(93) 0.15440(99) 0.2333(20) 1 0.802(84)
O1 O 0 0.55791(74) 0.15057(80) 0.4547(18) 1 0.802(84)
O2 O 0 0.63113(75) 0.31465(80) 0.2401(18) 1 0.802(84)
O3 O 0 0.3317(21) 0.3959(22) 0.4816(48) 1 0.802(84)
H1 D 0 0.4140(21) 0.2341(14) -0.0963(38) 1 0.96(10)
H2 D 0 0.4040(19) 0.4354(22) 0.0730(51) 1 0.96(10)
H3 D 0 0.2353(24) 0.3764(20) 0.0856(48) 1 0.96(10)
H4 D 0 0.2687(18) 0.1737(16) 0.4326(38) 1 0.96(10)
H5 D 0 0.2174(19) 0.1523(18) 0.1014(39) 1 0.96(10)
H6 D 0 0.3484(18) 0.0781(15) 0.2307(38) 1 0.96(10)
H7 D 0 0.2350(39) 0.3812(33) 0.5295(78) 1 0.96(10)
O4 O 0 0.07859(22) -0.00173(62) 0.32605(60) 1 0.802(84)
H8 D 0 0.0367(21) -0.0534(19) 0.1818(40) 1 0.96(10)
H9 D 0 0.0003(17) 0.0421(20) 0.4078(42) 1 0.96(10)

data_x_serhyI_45kbar.cif
_database_code_depnum_ccdc_archive 'CCDC 692791'

#Serine hydrate I at 4.5 GPa.
#Pure single crystal Xray refinement.
#Edinburgh dataset code = serhy4

_oxford_structure_analysis_title 'serhy4 in P2(1)2(1)2(1)'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   9.3728(5)
_cell_length_b                   11.0359(17)
_cell_length_c                   4.4782(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     463.21(8)

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

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 0.0010 0.0010 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'
N 0.0020 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0040 0.0030 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'

_cell_formula_units_Z            4

# Given Formula = C3 H9 N1 O4
# Dc = 1.77 Fooo = 264.00 Mu = 1.64 M = 123.11
# Found Formula = C3 H9 N1 O4
# Dc = 1.77 FOOO = 264.00 Mu = 1.64 M = 123.11

_chemical_formula_sum            'C3 H9 N1 O4'
_chemical_formula_moiety         'C3 H9 N1 O4'
_chemical_compound_source        ?
_chemical_formula_weight         123.11

_cell_measurement_reflns_used    730
_cell_measurement_theta_min      3
_cell_measurement_theta_max      18
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.10
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_max          0.20

_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_meas      ?
# Non-dispersive F(000):
_exptl_crystal_F_000             264
_exptl_absorpt_coefficient_mu    0.164

# Sheldrick geometric approximatio 0.97 0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.41
_exptl_absorpt_correction_T_max  0.98
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_type           ' synchrotron '
_diffrn_radiation_wavelength     0.48650
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_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_ambient_pressure         4500000
_diffrn_reflns_number            2738
_reflns_number_total             299
_diffrn_reflns_av_R_equivalents  0.1011
# Number of reflections with Friedels Law is 299
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 524
_diffrn_reflns_reduction_process 
;
Merged with SORTAV
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
;

_diffrn_reflns_theta_min         2.975
_diffrn_reflns_theta_max         18.333
_diffrn_measured_fraction_theta_max 0.460

_diffrn_reflns_theta_full        13.933
_diffrn_measured_fraction_theta_full 0.467

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       5
_reflns_limit_h_min              0
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              6
_reflns_limit_l_min              0
_reflns_limit_l_max              5

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

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

_refine_diff_density_min         -0.20
_refine_diff_density_max         0.22

_refine_ls_number_reflns         298
_refine_ls_number_restraints     85
_refine_ls_number_parameters     100

#_refine_ls_R_factor_ref 0.0465
_refine_ls_wR_factor_ref         0.0436
_refine_ls_goodness_of_fit_ref   0.8385

#_reflns_number_all 298
_refine_ls_R_factor_all          0.0465
_refine_ls_wR_factor_all         0.0436

# No actual I/u(I) cutoff was used for refinement. The
# threshold below is used for "_gt" information ONLY:
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                251
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_gt          0.0421

_refine_ls_shift/su_max          0.000121

# 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 Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    refxyz # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     
;
Method=
SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6)
;

_publ_section_exptl_refinement   
;
checkcif Output:

022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.46
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 13.93 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.47
089_ALERT_3_A Poor Data / Parameter Ratio (Zmax .LT. 18) ..... 2.98
910_ALERT_3_C # Missing FCF Reflections Below TH(Min) ........ 3
912_ALERT_3_C # Missing FCF Reflections Above STH/L=0.6 ...... 69
911_ALERT_3_B # Missing FCF Refl Between THmin & STh/l= 278

The high pressure cell causes shading of a significant proportion of the
sphere of reflections. This means that the completeness is reduced.

199_ALERT_1_A Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_A Check the Reported _diffrn_ambient_temperature . 293 K

Data were collected at 293K

042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?

The one given is chemically more meaningful

250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.55

This is probably due to the lack of information in one direction which occurs
as a result of the Merrill-Bassett diamond-anvil cell shading a significant
region of reciprocal space. The effect of this shading is often to cause a
smearing out of electron density in one particular direction.

731_ALERT_1_C Bond Calc 0.82(5), Rep 0.821(18) ...... 2.78 su-Rat
O4 -H8 1.555 1.555
731_ALERT_1_C Bond Calc 0.83(4), Rep 0.826(18) ...... 2.22 su-Rat
O4 -H9 1.555 1.555

This alert is due to the fact that PLATON calculates esds using only the
variances whereas CRYSTALS uses the full variance/covariance matrix.

;
# Insert your own references if required - in alphabetical order
_publ_section_references         
;
Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.

Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.

Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R.,
Munksgaard, Copenhagen, 291-294.

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

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

Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.

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
C1 C 0.54201(19) 0.2365(4) 0.2821(4) 0.0218 1.0000 Uani D U . . . .
C2 C 0.39741(18) 0.2470(4) 0.1279(4) 0.0219 1.0000 Uani D U . . . .
C3 C 0.33594(19) 0.3698(4) 0.1761(5) 0.0237 1.0000 Uani D U . . . .
N1 N 0.30095(15) 0.1515(5) 0.2388(4) 0.0238 1.0000 Uani D U . . . .
O1 O 0.56151(14) 0.1490(4) 0.4485(5) 0.0420 1.0000 Uani D U . . . .
O2 O 0.63011(13) 0.3198(4) 0.2343(3) 0.0278 1.0000 Uani D U . . . .
O3 O 0.33259(15) 0.3969(4) 0.4859(3) 0.0314 1.0000 Uani D U . . . .
O4 O 0.07828(15) -0.0024(4) 0.3199(5) 0.0253 1.0000 Uani D . . . . .
H1 H 0.4134(18) 0.236(2) -0.085(3) 0.0276 1.0000 Uiso D . . . . .
H2 H 0.394(2) 0.430(2) 0.077(4) 0.0289 1.0000 Uiso D . . . . .
H3 H 0.2403(16) 0.371(2) 0.098(4) 0.0289 1.0000 Uiso D . . . . .
H4 H 0.278(2) 0.166(2) 0.430(4) 0.0362 1.0000 Uiso D . . . . .
H5 H 0.2230(19) 0.150(3) 0.126(4) 0.0362 1.0000 Uiso D . . . . .
H6 H 0.344(2) 0.0797(18) 0.227(6) 0.0362 1.0000 Uiso D . . . . .
H7 H 0.257(3) 0.363(5) 0.529(8) 0.0460 1.0000 Uiso D . . . . .
H8 H 0.037(4) -0.043(6) 0.193(9) 0.0523 1.0000 Uiso D . . . . .
H9 H 0.011(3) 0.033(6) 0.401(9) 0.0523 1.0000 Uiso D . . . . .
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
C1 0.0150(7) 0.038(4) 0.0123(9) 0.0026(16) 0.0025(7) 0.0001(13)
C2 0.0159(8) 0.035(4) 0.0146(8) -0.0018(16) 0.0012(6) 0.0006(14)
C3 0.0173(8) 0.032(4) 0.0222(9) 0.0012(17) 0.0001(6) -0.0021(16)
N1 0.0163(6) 0.034(5) 0.0208(8) -0.0011(16) -0.0017(6) -0.0031(14)
O1 0.0180(6) 0.055(5) 0.0527(11) 0.030(2) -0.0067(7) -0.0094(16)
O2 0.0189(6) 0.043(4) 0.0214(7) 0.0039(12) 0.0018(5) -0.0055(11)
O3 0.0185(6) 0.049(5) 0.0269(8) -0.0128(14) 0.0060(5) -0.0065(13)
O4 0.0258(7) 0.020(6) 0.0300(8) 0.0022(14) -0.0019(6) 0.0010(12)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          3.15(9)
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 . C2 . 1.526(2) yes
C1 . O1 . 1.233(5) yes
C1 . O2 . 1.255(4) yes
C2 . C3 . 1.488(6) yes
C2 . N1 . 1.475(5) yes
C2 . H1 . 0.973(15) no
C3 . O3 . 1.419(3) yes
C3 . H2 . 0.968(17) no
C3 . H3 . 0.962(15) no
N1 . H4 . 0.896(16) no
N1 . H5 . 0.889(16) no
N1 . H6 . 0.888(17) no
O3 . H7 . 0.826(17) no
O4 . H8 . 0.821(18) no
O4 . H9 . 0.826(18) 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
C2 . C1 . O1 . 117.7(2) yes
C2 . C1 . O2 . 116.8(2) yes
O1 . C1 . O2 . 125.42(18) yes
C1 . C2 . C3 . 110.4(2) yes
C1 . C2 . N1 . 109.7(2) yes
C3 . C2 . N1 . 111.40(18) yes
C1 . C2 . H1 . 107.3(10) no
C3 . C2 . H1 . 108.1(14) no
N1 . C2 . H1 . 109.8(13) no
C2 . C3 . O3 . 110.0(2) yes
C2 . C3 . H2 . 110.2(13) no
O3 . C3 . H2 . 108.4(12) no
C2 . C3 . H3 . 108.7(15) no
O3 . C3 . H3 . 109.4(11) no
H2 . C3 . H3 . 110.1(14) no
C2 . N1 . H4 . 109.5(15) no
C2 . N1 . H5 . 109.1(14) no
H4 . N1 . H5 . 110.8(14) no
C2 . N1 . H6 . 110.0(13) no
H4 . N1 . H6 . 109.1(16) no
H5 . N1 . H6 . 108.4(16) no
C3 . O3 . H7 . 99(3) no
H8 . O4 . H9 . 102(4) no
_chemical_name_common            'Serine Monohydrate'
_exptl_crystal_recrystallization_method 'From H2O/EtOH'

data_x_serhyII_52kbar
_database_code_depnum_ccdc_archive 'CCDC 692792'

#Serine hydrate phase II at 5.2 GPa.
#X-N refinement. #X-N refinement. Xray data set is x_serhyII_52kbar.
#Edinburgh dataset code = serhy5

#Notes on this cif:
#The structural data comes from a joint X-N refinement (see text in paper)
#The majority of this cif was generated with CRYSTALS.
#The Topas cif was processed using Platon so that x's and u's conform to the
#'rule of 19'. The x's, u's and geometrical parameters were then pasted into
#this cif. R-factors: _refine_ls_wR_factor_ref corresponds to the Topas Rwp.
#Other R-factors were calculated by importing the final model into crystals
#and doing a structure factor calculation.

_oxford_structure_analysis_title 'serhy5 in P2(1)2(1)2(1)'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   9.8778(13)
_cell_length_b                   10.155(4)
_cell_length_c                   4.4175(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     443.13(18)

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

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 0.0010 0.0010 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'
N 0.0020 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0040 0.0030 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'

_cell_formula_units_Z            4

# Given Formula = C3 H9 N1 O4
# Dc = 1.85 Fooo = 264.00 Mu = 1.71 M = 123.11
# Found Formula = C3 H9 N1 O4
# Dc = 1.85 FOOO = 264.00 Mu = 1.71 M = 123.11

_chemical_formula_sum            'C3 H9 N1 O4'
_chemical_formula_moiety         'C3 H9 N1 O4'
_chemical_compound_source        ?
_chemical_formula_weight         123.11

_cell_measurement_reflns_used    542
_cell_measurement_theta_min      3
_cell_measurement_theta_max      17
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.10
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_max          0.20

_exptl_crystal_density_diffrn    1.845
_exptl_crystal_density_meas      ?
# Non-dispersive F(000):
_exptl_crystal_F_000             264
_exptl_absorpt_coefficient_mu    0.171

# Sheldrick geometric approximatio 0.97 0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_T_max  0.98
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_type           ' synchrotron '
_diffrn_radiation_wavelength     0.48650
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_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_ambient_pressure         5200000
_diffrn_reflns_number            2207
_reflns_number_total             276
_diffrn_reflns_av_R_equivalents  0.1768
# Number of reflections with Friedels Law is 276
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 455
_diffrn_reflns_reduction_process 
;
Merged with SORTAV
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
;

_diffrn_reflns_theta_min         2.823
_diffrn_reflns_theta_max         17.722
_diffrn_measured_fraction_theta_max 0.484

_diffrn_reflns_theta_full        15.063
_diffrn_measured_fraction_theta_full 0.492

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       5
_reflns_limit_h_min              0
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              6
_reflns_limit_l_min              0
_reflns_limit_l_max              5

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

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

_refine_diff_density_min         -0.36
_refine_diff_density_max         0.29

_refine_ls_number_reflns         246
_refine_ls_number_restraints     3
_refine_ls_number_parameters     109 #in full x-n refinement

_refine_ls_wR_factor_ref         0.1110
_refine_ls_goodness_of_fit_ref   1.670

#_reflns_number_all 253
_refine_ls_R_factor_all          0.1128
_refine_ls_wR_factor_all         0.1110

# No actual I/u(I) cutoff was used for refinement. The
# threshold below is used for "_gt" information ONLY:
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                167
_refine_ls_R_factor_gt           0.0718
_refine_ls_wR_factor_gt          0.1032

_refine_ls_shift/su_max          0.000

# 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 Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?

_publ_section_exptl_refinement   
;
Checkcif Output:

022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.49
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 15.06 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.49
089_ALERT_3_A Poor Data / Parameter Ratio (Zmax .LT. 18) ..... 2.26

020_ALERT_3_B The value of Rint is greater than 0.10 ......... 0.18

250_ALERT_2_B Large U3/U1 Ratio for Average U(i,j) Tensor .... 6.35
213_ALERT_2_C Atom C2 has ADP max/min Ratio ............. 3.10 prola

The TLS formalism was used to constarin the Uijs. The lack of data in one
direction of reciprocal space (due to the pressure cell) will distirt these
tensors, though the distortion is not as great as on full independent Uij
refinement.

340_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 13

This calculation does not take the off diagonal variance-covariance terms
into account. See text.

417_ALERT_2_B Short Inter D-H..H-D H6 .. H8 .. 2.06 Ang.
415_ALERT_2_C Short Inter D-H..H-X H2 .. H9 .. 2.12 Ang.

This is a high-pressure crystal structure. H...H distances can fall as low as
1.7 Ang.

042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
No action.

125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?

No action.

152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?

Just a rounding error:
Volume Reported 443.13(18) Calculated 443.1(2)

245_ALERT_2_C U(iso) H4 Smaller than U(eq) N1 by ... 0.01 AngSq
245_ALERT_2_C U(iso) H5 Smaller than U(eq) N1 by ... 0.01 AngSq
245_ALERT_2_C U(iso) H6 Smaller than U(eq) N1 by ... 0.01 AngSq
245_ALERT_2_C U(iso) H7 Smaller than U(eq) O3 by ... 0.01 AngSq

No action.

199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
791_ALERT_1_G Confirm the Absolute Configuration of C2 = . S
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 3

All OK.

;

# Insert your own references if required - in alphabetical order
_publ_section_references         
;
Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.

Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.

Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R.,
Munksgaard, Copenhagen, 291-294.

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

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

Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.

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_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
O1 O Uani 0.6052(9) 0.1840(11) 0.489(2) 1.000 0.043(4) . .
O2 O Uani 0.6580(10) 0.3339(11) 0.139(2) 1.000 0.043(4) . .
O3 O Uani 0.348(3) 0.416(3) 0.487(6) 1.000 0.044(4) . .
N1 N Uani 0.3572(11) 0.1445(16) 0.292(3) 1.000 0.043(3) . .
C1 C Uani 0.5769(3) 0.2564(5) 0.2663(7) 1.000 0.038(3) . .
C2 C Uani 0.4336(5) 0.2507(12) 0.1385(16) 1.000 0.037(3) . .
C3 C Uani 0.3633(14) 0.384(2) 0.173(4) 1.000 0.040(3) . .
O4 O Uani 0.0869(3) 0.0103(8) 0.3104(11) 1.000 0.024(5) . .
H1 H Uiso 0.433(2) 0.228(2) -0.079(5) 1.000 0.030(9) . .
H2 H Uiso 0.420(2) 0.451(3) 0.072(6) 1.000 0.030(9) . .
H3 H Uiso 0.274(3) 0.377(3) 0.077(6) 1.000 0.030(9) . .
H4 H Uiso 0.273(2) 0.177(3) 0.360(5) 1.000 0.030(9) . .
H5 H Uiso 0.342(2) 0.075(3) 0.158(5) 1.000 0.030(9) . .
H6 H Uiso 0.406(2) 0.1135(19) 0.460(4) 1.000 0.030(9) . .
H7 H Uiso 0.270(4) 0.383(4) 0.538(9) 1.000 0.030(9) . .
H8 H Uiso 0.108(2) 0.067(2) 0.168(5) 1.000 0.030(9) . .
H9 H Uiso 0.005(2) 0.032(2) 0.366(4) 1.000 0.030(9) . .

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
O1 0.013(3) 0.099(12) 0.018(5) 0.005(5) -0.003(3) -0.005(3)
O2 0.016(2) 0.086(10) 0.026(8) 0.001(6) 0.003(3) -0.005(3)
O3 0.016(4) 0.096(10) 0.021(7) -0.017(5) -0.003(4) -0.005(4)
N1 0.018(3) 0.087(8) 0.025(5) -0.004(5) -0.007(3) -0.010(3)
C1 0.0139(18) 0.084(8) 0.015(4) -0.002(4) -0.002(2) -0.005(2)
C2 0.016(2) 0.083(8) 0.012(3) -0.006(3) -0.004(2) -0.004(3)
C3 0.017(2) 0.086(9) 0.017(5) -0.005(4) 0.000(3) 0.000(3)
O4 0.0220(17) 0.029(16) 0.022(3) 0.005(4) 0.0032(17) 0.006(3)

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
O1 C1 1.260(10) . . yes
O2 C1 1.256(11) . . yes
O3 C3 1.43(3) . . yes
O3 H7 0.87(5) . . no
O4 H9 0.87(2) . . no
O4 H8 0.88(2) . . no
N1 C2 1.481(17) . . yes
N1 H5 0.93(3) . . no
N1 H4 0.94(2) . . no
N1 H6 0.94(2) . . no
C1 C2 1.525(6) . . no
C2 C3 1.53(2) . . no
C2 H1 0.99(2) . . no
C3 H3 0.98(3) . . no
C3 H2 0.99(3) . . no

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
C3 O3 H7 105(4) . . . no
H8 O4 H9 104.8(19) . . . no
C2 N1 H5 110.0(19) . . . no
C2 N1 H6 110.1(16) . . . no
H4 N1 H5 109(2) . . . no
H4 N1 H6 109(2) . . . no
H5 N1 H6 109(3) . . . no
C2 N1 H4 110(2) . . . no
O1 C1 O2 125.0(7) . . . yes
O2 C1 C2 116.8(6) . . . yes
O1 C1 C2 118.2(6) . . . yes
N1 C2 C1 109.3(7) . . . yes
N1 C2 C3 111.6(9) . . . yes
C1 C2 C3 110.6(9) . . . no
O3 C3 C2 110.2(17) . . . yes
N1 C2 H1 105.8(15) . . . no
C3 C2 H1 107.5(15) . . . no
C1 C2 H1 112.0(12) . . . no
O3 C3 H2 110(3) . . . no
O3 C3 H3 110(2) . . . no
C2 C3 H3 108(2) . . . no
H2 C3 H3 111(3) . . . no
C2 C3 H2 107.9(19) . . . no

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
O1 C1 C2 N1 -6.3(11) . . . . no
O1 C1 C2 C3 116.9(10) . . . . no
O2 C1 C2 N1 173.7(9) . . . . no
O2 C1 C2 C3 -63.1(10) . . . . no
N1 C2 C3 O3 58.3(18) . . . . no
C1 C2 C3 O3 -63.6(17) . . . . no

_chemical_name_common            'Serine Monohydrate'
_exptl_crystal_recrystallization_method 'From H2O/EtOH'

data_n_serhyII_58kbar
_database_code_depnum_ccdc_archive 'CCDC 692793'

#Serine hydrate phase II at 5.8 GPa.
#X-N refinement.
#Structural parameters here model the neutron powder data set.
#ISIS data set code: PRL57157_66_60TNS_ASCII_TOF

_chemical_name_systematic        
;
perdeuterated L-serine hydrate
;
_chemical_name_common            'Serine hydrate'

_chemical_formula_moiety         'C3 D7 N O3, D2 O1'
_chemical_formula_structural     ?
_chemical_formula_sum            'C3 D9 N O4'
_chemical_formula_weight         132.13
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P212121
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_Int_Tables_number      19

_cell_length_a                   9.8641(14)
_cell_length_b                   10.09910(93)
_cell_length_c                   4.39860(65)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     438.18(10)

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

_cell_measurement_temperature    298
_cell_measurement_pressure       5810000 #5.810(11) GPa
_cell_measurement_reflns_used    1034
_cell_formula_units_Z            4

_cell_special_details            
;
Cell parameters included in refinement
;
_exptl_crystal_density_diffrn    2.003
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             ?

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_particle_morphology     Block
_pd_char_colour                  Colourless
_chemical_absolute_configuration rm

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS software.
;

_pd_instr_location               'ISIS, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      298
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            ?
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'HiPr/PEARL, ISIS'
_diffrn_radiation_monochromator  ?
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom
_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source

;

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_number            1034

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

_pd_instr_dist_src/spec          12600
_pd_instr_dist_spec/detc         600
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
Modelling of preferred orientation was found to be unnecessary.
;

_pd_proc_ls_prof_R_factor        1.829
_pd_proc_ls_prof_wR_factor       1.484
_pd_proc_ls_prof_R_expected      1.226
_refine_ls_goodness_of_fit_all   1.211

_refine_ls_matrix_type           sparse
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     109
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          <0.001

_pd_proc_info_excluded_regions   
;
excluded short TOF region above

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;

Refinement was carried out against neutron and X-ray data simultaneously.
The X-ray data had been collected using synchrotron radiation, and the
pressure (ruby fluorescence) was 3.7 GPa. wR2 = 11.103 and S = 1.670 for
pure 1/sigma^2 weights.

Checkcif output:
023_ALERT_3_A Resolution (too) Low [sin(th)/Lambda < 0.6]..... 0.00 Deg.
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 0.00 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.00
037_ALERT_1_A _diffrn_reflns_theta_full .......... Not Given . ?
038_ALERT_1_A _diffrn_measured_fraction_theta_max Not Given . ?
039_ALERT_1_A _diffrn_measured_fraction_theta_full Not Given . ?

The resolution range was 0.64 to 4.14 Ang.

050_ALERT_1_A Absorption Coefficient mu Missing .............. ?

TOF data - the absorption coefficient is variable.

095_ALERT_1_A No Residual Density Maximum Given .............. ?
096_ALERT_1_A No Residual Density Minimum Given .............. ?

These data are not yet output by TOPAS.

201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8
210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ?

Powder data: see text of paper.

340_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 13

This is quite good for a high pressure neutron powder refinement!

415_ALERT_2_B Short Inter D-H..H-X H2 .. H8 .. 2.08 Ang.
415_ALERT_2_B Short Inter D-H..H-X H2 .. H9 .. 2.04 Ang.
417_ALERT_2_B Short Inter D-H..H-D H4 .. H8 .. 2.09 Ang.
417_ALERT_2_B Short Inter D-H..H-D H6 .. H8 .. 2.01 Ang.
432_ALERT_2_C Short Inter X...Y Contact O4 .. C1 .. 3.01 Ang.
432_ALERT_2_C Short Inter X...Y Contact O4 .. C2 .. 3.01 Ang.

This is a high pressure structure. H...H contacts may be as short as 1.7 Ang
in structures below 10 GPa.

040_ALERT_1_C No H-atoms in this Carbon Containing Compound .. ?
720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 9

The sample was deuterated.

152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?

A rounding error:
Volume Reported 438.18(10) Calculated 438.18(9)
;

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
C1 C 0 0.57685(32) 0.25635(53) 0.26630(67) 1 1.254(89)
C2 C 0 0.43359(49) 0.2507(12) 0.1385(16) 1 1.254(89)
C3 C 0 0.3633(14) 0.3839(22) 0.1730(40) 1 1.254(89)
N1 N 0 0.3572(11) 0.1445(16) 0.2922(26) 1 1.254(89)
O1 O 0 0.60520(93) 0.1840(11) 0.4892(22) 1 1.254(89)
O2 O 0 0.65801(97) 0.3339(11) 0.1387(23) 1 1.254(89)
O3 O 0 0.3484(26) 0.4155(31) 0.4868(63) 1 1.254(89)
H1 D 0 0.4329(25) 0.2255(21) -0.1003(43) 1 1.50(11)
H2 D 0 0.4251(23) 0.4578(28) 0.0618(60) 1 1.50(11)
H3 D 0 0.2648(27) 0.3768(30) 0.0666(59) 1 1.50(11)
H4 D 0 0.2647(19) 0.1797(24) 0.3670(44) 1 1.50(11)
H5 D 0 0.3403(19) 0.0668(23) 0.1443(43) 1 1.50(11)
H6 D 0 0.4110(19) 0.1096(18) 0.4771(40) 1 1.50(11)
H7 D 0 0.2611(44) 0.3804(43) 0.5446(93) 1 1.50(11)
O4 O 0 0.08688(34) 0.01031(79) 0.3104(11) 1 1.254(89)
H8 D 0 0.1104(21) 0.0727(21) 0.1525(46) 1 1.50(11)
H9 D 0 -0.0037(16) 0.0347(19) 0.3725(48) 1 1.50(11)


