# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_n-dodecane
_database_code_depnum_ccdc_archive 'CCDC 2281143'
loop_
_audit_author_name
_audit_author_address
'Tomasz Poreba'
;European Synchrotron Radiation Facility
France
;
_audit_update_record             
;
2023-07-12 deposited with the CCDC.	2023-11-03 downloaded from the CCDC.
;
_audit_creation_date             2023-07-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2017/1
loop_
_audit_author_email
tomasz.poreba@esrf.fr
_chemical_name_common            dodecane
_chemical_name_systematic        n-dodecane
_chemical_formula_moiety         'C12 H26'
_chemical_formula_sum            'C12 H26'
_chemical_formula_weight         170.33
_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 -0.0011 0.0005 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   4.2522(9)
_cell_length_b                   4.7701(11)
_cell_length_c                   15.904(6)
_cell_angle_alpha                88.90(3)
_cell_angle_beta                 84.67(2)
_cell_angle_gamma                73.309(19)
_cell_volume                     307.64(16)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1339
_cell_measurement_temperature    295
_cell_measurement_pressure       150000
_cell_measurement_theta_max      18.375
_cell_measurement_theta_min      2.226
_shelx_estimated_absorpt_T_max   0.999
_shelx_estimated_absorpt_T_min   0.994
_exptl_absorpt_coefficient_mu    0.025
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.919
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             98
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.436
_diffrn_reflns_Laue_measured_fraction_max 0.354
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            1339
_diffrn_reflns_point_group_measured_fraction_full 0.436
_diffrn_reflns_point_group_measured_fraction_max 0.354
_diffrn_reflns_theta_full        14.241
_diffrn_reflns_theta_max         18.375
_diffrn_reflns_theta_min         2.226
_diffrn_ambient_temperature      295(1)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.436
_diffrn_measured_fraction_theta_max 0.354
_diffrn_ambient_pressure         150000
_diffrn_ambient_environment      Helium
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            'Eiger 9M CdTe'
_diffrn_measurement_specimen_suport 'diamond anvil cell'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_exptl_special_details           
;
Data were collected at room temperature and pressure of 0.15(3) GPa
(150000 kPa).Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
;
_diffrn_measurement_method       'omega scan'
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
Two of these runs were performed for two crystals in two different orientations.
Then, the two datasets were merged in SORTAV
;
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.410
_diffrn_source                   synchrotron
_diffrn_radiation_probe          x-ray
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                439
_reflns_number_total             834
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.075
_refine_diff_density_min         -0.074
_refine_diff_density_rms         0.022
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         834
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0662
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1497P)²+0.0002P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2262
_refine_ls_wR_factor_ref         0.2574
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C5 C 0.2185(3) 0.3604(5) 0.38804(7) 0.0582(8) Uani 1 1 d . . . . .
H5A H 0.076805 0.242449 0.375498 0.070 Uiso 1 1 calc R U . . .
H5B H 0.419003 0.230054 0.407029 0.070 Uiso 1 1 calc R U . . .
C6 C 0.0442(3) 0.5767(5) 0.45930(7) 0.0584(8) Uani 1 1 d . . . . .
H6A H -0.156021 0.707376 0.440263 0.070 Uiso 1 1 calc R U . . .
H6B H 0.186125 0.694374 0.471931 0.070 Uiso 1 1 calc R U . . .
C4 C 0.3059(3) 0.5133(5) 0.30688(8) 0.0600(8) Uani 1 1 d . . . . .
H4A H 0.105024 0.643007 0.287854 0.072 Uiso 1 1 calc R U . . .
H4B H 0.446208 0.632328 0.319622 0.072 Uiso 1 1 calc R U . . .
C3 C 0.4813(3) 0.3000(5) 0.23559(8) 0.0591(9) Uani 1 1 d . . . . .
H3A H 0.341383 0.180283 0.223139 0.071 Uiso 1 1 calc R U . . .
H3B H 0.682585 0.170985 0.254593 0.071 Uiso 1 1 calc R U . . .
C1 C 0.7443(4) 0.2356(6) 0.08443(9) 0.0838(11) Uani 1 1 d . . . . .
H1A H 0.941683 0.106122 0.103612 0.126 Uiso 1 1 calc R U . . .
H1B H 0.800448 0.341051 0.036064 0.126 Uiso 1 1 calc R U . . .
H1C H 0.602652 0.123815 0.069301 0.126 Uiso 1 1 calc R U . . .
C2 C 0.5674(4) 0.4506(6) 0.15453(8) 0.0703(9) Uani 1 1 d . . . . .
H2A H 0.366137 0.578187 0.135084 0.084 Uiso 1 1 calc R U . . .
H2B H 0.706167 0.571456 0.166919 0.084 Uiso 1 1 calc R U . . .

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
C5 0.0670(9) 0.054(2) 0.0473(8) -0.0053(12) 0.0046(7) -0.0109(8)
C6 0.0654(8) 0.056(2) 0.0480(9) -0.0077(13) 0.0056(7) -0.0112(7)
C4 0.0671(8) 0.058(2) 0.0483(8) -0.0051(12) 0.0053(7) -0.0104(8)
C3 0.0679(9) 0.056(2) 0.0476(8) -0.0038(13) 0.0047(6) -0.0118(8)
C1 0.0917(11) 0.096(3) 0.0543(9) -0.0082(15) 0.0150(7) -0.0179(12)
C2 0.0785(9) 0.074(2) 0.0509(8) -0.0027(12) 0.0080(7) -0.0148(9)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.532(2) . ?
C5 C4 1.538(3) . ?
C6 C6 1.544(4) 2_566 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.526(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.530(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C2 1.518(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 109.0 . . ?
C6 C5 H5B 109.0 . . ?
C6 C5 C4 112.8(2) . . ?
C4 C5 H5A 109.0 . . ?
C4 C5 H5B 109.0 . . ?
C5 C6 C6 112.8(3) . 2_566 ?
C5 C6 H6A 109.0 . . ?
C5 C6 H6B 109.0 . . ?
C6 C6 H6A 109.0 2_566 . ?
C6 C6 H6B 109.0 2_566 . ?
H6A C6 H6B 107.8 . . ?
C5 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
C3 C4 C5 113.3(2) . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
C4 C3 H3A 108.9 . . ?
C4 C3 H3B 108.9 . . ?
C4 C3 C2 113.5(2) . . ?
H3A C3 H3B 107.7 . . ?
C2 C3 H3A 108.9 . . ?
C2 C3 H3B 108.9 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C3 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
C1 C2 C3 112.9(2) . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?

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
C5 C4 C3 C2 179.70(10) . . . . ?
C6 C5 C4 C3 179.68(9) . . . . ?
C4 C5 C6 C6 179.87(12) . . . 2_566 ?
C4 C3 C2 C1 179.52(11) . . . . ?

_shelx_res_file                  
;
TITL 0016_0001_a.res in P-1
    n-dodecane.res
    created by SHELXL-2017/1 at 16:33:40 on 12-Jul-2023
CELL 0.41 4.252157 4.770067 15.903911 88.9005 84.6716 73.309
ZERR 1 0.000855 0.001141 0.00634 0.026 0.0238 0.0193
LATT 1
SFAC C H
DISP C -0.0011 0.0005 5.0796
DISP H 0 0 0.5971
UNIT 12 26
EQIV $1 2-X,-Y,-Z

L.S. 4 0 0
PLAN  4
SIZE 0.05 0.07 0.25
TEMP 21.85
CONF
FREE C1 C1_$1
MORE -1
BOND $H
fmap 2 53
acta
SHEL 0.65 1000
REM <olex2.extras>
REM <HklSrc "%.\\unmerged.hkl">
REM </olex2.extras>

WGHT    0.149700    0.000200
FVAR       4.73665
C5    1    0.218502    0.360427    0.388037    11.00000    0.06703    0.05440 =
         0.04730   -0.00532    0.00456   -0.01089
AFIX  23
H5A   2    0.076805    0.242449    0.375498    11.00000   -1.20000
H5B   2    0.419003    0.230054    0.407029    11.00000   -1.20000
AFIX   0
C6    1    0.044211    0.576708    0.459302    11.00000    0.06544    0.05610 =
         0.04795   -0.00773    0.00560   -0.01117
AFIX  23
H6A   2   -0.156021    0.707376    0.440263    11.00000   -1.20000
H6B   2    0.186125    0.694374    0.471931    11.00000   -1.20000
AFIX   0
C4    1    0.305867    0.513322    0.306878    11.00000    0.06712    0.05794 =
         0.04834   -0.00513    0.00531   -0.01038
AFIX  23
H4A   2    0.105024    0.643007    0.287854    11.00000   -1.20000
H4B   2    0.446208    0.632328    0.319622    11.00000   -1.20000
AFIX   0
C3    1    0.481320    0.300014    0.235590    11.00000    0.06790    0.05618 =
         0.04758   -0.00379    0.00470   -0.01184
AFIX  23
H3A   2    0.341383    0.180283    0.223139    11.00000   -1.20000
H3B   2    0.682585    0.170985    0.254593    11.00000   -1.20000
AFIX   0
C1    1    0.744302    0.235635    0.084433    11.00000    0.09166    0.09576 =
         0.05432   -0.00818    0.01500   -0.01792
AFIX 137
H1A   2    0.941683    0.106122    0.103612    11.00000   -1.50000
H1B   2    0.800448    0.341051    0.036064    11.00000   -1.50000
H1C   2    0.602652    0.123815    0.069301    11.00000   -1.50000
AFIX   0
C2    1    0.567351    0.450610    0.154533    11.00000    0.07854    0.07441 =
         0.05092   -0.00267    0.00798   -0.01481
AFIX  23
H2A   2    0.366137    0.578187    0.135084    11.00000   -1.20000
H2B   2    0.706167    0.571456    0.166919    11.00000   -1.20000
AFIX   0
HKLF 4




REM  0016_0001_a.res in P-1
REM R1 =  0.0662 for     439 Fo > 4sig(Fo)  and  0.0953 for all     834 data
REM     56 parameters refined using      0 restraints

END

WGHT      0.1497      0.0002

REM Highest difference peak  0.075,  deepest hole -0.074,  1-sigma level  0.022
Q1    1   0.1421  0.4533  0.4225  11.00000  0.05    0.08
Q2    1   0.5000  0.5000  0.5000  10.50000  0.05    0.07
Q3    1   0.5058  0.5592  0.2191  11.00000  0.05    0.07
Q4    1   0.2723  0.5795  0.3775  11.00000  0.05    0.07
;
_shelx_res_checksum              51288
_olex2_exptl_crystal_mounting_method DAC
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT029_n-dodecane          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.436 Why?  
RESPONSE: Sample was measured in diamond anvil cell, which geometry limits
	access to full Ewald sphere
;
_vrf_PLAT049_n-dodecane          
;
PROBLEM: Calculated Density Less Than 1.0 gcm-3 .........     0.9194 Check 
RESPONSE: It is typical for crystals of low n-alkanes
;
_vrf_PLAT911_n-dodecane          
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        626 Report
RESPONSE: It is due to geometrical restraints of diamond anvil cell
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 
'isochoric recrystallization at high pressure in diamond anvil cell'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_undecane
_database_code_depnum_ccdc_archive 'CCDC 2281144'
loop_
_audit_author_name
_audit_author_address
'Tomasz Poreba'
;European Synchrotron Radiation Facility
France
;
_audit_update_record             
;
2023-07-12 deposited with the CCDC.	2023-11-03 downloaded from the CCDC.
;
_audit_creation_date             2023-07-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2017/1
loop_
_audit_author_email
tomasz.poreba@esrf.fr
_chemical_name_common            undecane
_chemical_name_systematic        n-undecane
_chemical_formula_moiety         'C11 H24'
_chemical_formula_sum            'C11 H24'
_chemical_formula_weight         156.30
_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 -0.0011 0.0005 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   4.1808(5)
_cell_length_b                   4.7113(3)
_cell_length_c                   29.53(2)
_cell_angle_alpha                93.609(19)
_cell_angle_beta                 90.41(2)
_cell_angle_gamma                107.274(9)
_cell_volume                     554.1(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    147
_cell_measurement_temperature    295
_cell_measurement_pressure       170000
_cell_measurement_theta_max      16.1090
_cell_measurement_theta_min      2.6160
_shelx_estimated_absorpt_T_max   0.999
_shelx_estimated_absorpt_T_min   0.994
_exptl_absorpt_coefficient_mu    0.025
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58199
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.937
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             180
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0054
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_Laue_measured_fraction_full 0.268
_diffrn_reflns_Laue_measured_fraction_max 0.261
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            867
_diffrn_reflns_point_group_measured_fraction_full 0.268
_diffrn_reflns_point_group_measured_fraction_max 0.261
_diffrn_reflns_theta_full        14.241
_diffrn_reflns_theta_max         14.802
_diffrn_reflns_theta_min         2.618
_diffrn_ambient_temperature      295
_diffrn_ambient_pressure         170000
_diffrn_ambient_environment      Helium
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            'Eiger 9M CdTe'
_diffrn_measurement_specimen_suport 'diamond anvil cell'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'

_exptl_special_details           
;
Data were collected at room temperature and pressure of 0.17(3) GPa
(170000 kPa).Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
;
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.268
_diffrn_measured_fraction_theta_max 0.261
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'

_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0134237000
_diffrn_orient_matrix_UB_12      0.0048137000
_diffrn_orient_matrix_UB_13      0.0137352000
_diffrn_orient_matrix_UB_21      -0.0273326000
_diffrn_orient_matrix_UB_22      -0.0911428000
_diffrn_orient_matrix_UB_23      -0.0001327000
_diffrn_orient_matrix_UB_31      0.0981195000
_diffrn_orient_matrix_UB_32      0.0037707000
_diffrn_orient_matrix_UB_33      0.0022379000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.410
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                253
_reflns_number_total             586
_reflns_odcompleteness_completeness 15.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     21.01
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.072
_refine_diff_density_min         -0.070
_refine_diff_density_rms         0.023
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         586
_refine_ls_number_restraints     80
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0539
_refine_ls_restrained_S_all      0.972
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1112P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1951
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C11-C10 = C9-C10 = C9-C8 = C8-C7 = C7-C6 = C6-C5 = C5-C4 = C4-C3 = C3-C2 = C2-
 C1
 1.52 with sigma of 0.005
 C1-C2 \\sim C2-C3
 with sigma of 0.02
 C9-C10 \\sim C10-C11
 with sigma of 0.02
 C3-C4 \\sim C4-C5
 with sigma of 0.02
 C5-C6 \\sim C6-C7
 with sigma of 0.02
 C7-C8 \\sim C8-C9
 with sigma of 0.02
 C9-C8 \\sim C8-C7
 with sigma of 0.02
 C7-C6 \\sim C7-C8
 with sigma of 0.02
 C10-C9 \\sim C9-C8
 with sigma of 0.02
 C5-C6 \\sim C5-C4
 with sigma of 0.02
 C3-C4 \\sim C2-C3
 with sigma of 0.02
3. Rigid bond restraints
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C4(H4A,H4B), C8(H8A,H8B), C3(H3A,H3B), C9(H9A,H9B), C10(H10A,
 H10B), C7(H7A,H7B), C5(H5A,H5B), C2(H2A,H2B)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C6 C 0.2606(8) 0.5578(7) 0.7458(2) 0.053(4) Uani 1 1 d D U . . .
H6A H 0.045131 0.419585 0.736254 0.063 Uiso 1 1 calc R U . . .
H6B H 0.408819 0.441190 0.752688 0.063 Uiso 1 1 calc R U . . .
C4 C 0.4489(8) 0.5739(7) 0.6639(2) 0.058(4) Uani 1 1 d D U . . .
H4A H 0.233964 0.435730 0.654053 0.069 Uiso 1 1 calc R U . . .
H4B H 0.596829 0.456997 0.670734 0.069 Uiso 1 1 calc R U . . .
C8 C 0.0760(8) 0.5453(8) 0.8278(2) 0.057(4) Uani 1 1 d D U . . .
H8A H -0.140121 0.407167 0.818378 0.068 Uiso 1 1 calc R U . . .
H8B H 0.224040 0.428623 0.834638 0.068 Uiso 1 1 calc R U . . .
C3 C 0.5915(8) 0.7619(7) 0.6250(2) 0.055(4) Uani 1 1 d D U . . .
H3A H 0.806955 0.899292 0.634783 0.066 Uiso 1 1 calc R U . . .
H3B H 0.444290 0.879819 0.618296 0.066 Uiso 1 1 calc R U . . .
C9 C 0.0335(8) 0.7221(7) 0.8703(3) 0.057(4) Uani 1 1 d D U . . .
H9A H -0.116263 0.837285 0.863503 0.069 Uiso 1 1 calc R U . . .
H9B H 0.249200 0.861696 0.879514 0.069 Uiso 1 1 calc R U . . .
C10 C -0.1029(10) 0.5371(9) 0.9097(3) 0.069(4) Uani 1 1 d D U . . .
H10A H 0.045510 0.420334 0.916375 0.083 Uiso 1 1 calc R U . . .
H10B H -0.319781 0.399108 0.900694 0.083 Uiso 1 1 calc R U . . .
C7 C 0.2156(8) 0.7317(7) 0.7886(2) 0.053(4) Uani 1 1 d D U . . .
H7A H 0.067030 0.847894 0.781785 0.063 Uiso 1 1 calc R U . . .
H7B H 0.431074 0.870378 0.798145 0.063 Uiso 1 1 calc R U . . .
C5 C 0.4011(7) 0.7449(7) 0.7069(2) 0.054(4) Uani 1 1 d D U . . .
H5A H 0.615858 0.883800 0.716653 0.065 Uiso 1 1 calc R U . . .
H5B H 0.252284 0.860960 0.700097 0.065 Uiso 1 1 calc R U . . .
C1 C 0.7868(11) 0.7822(8) 0.5427(3) 0.074(5) Uani 1 1 d D U . . .
H1A H 0.816059 0.656339 0.517242 0.112 Uiso 1 1 calc R U . . .
H1B H 0.999874 0.918853 0.552348 0.112 Uiso 1 1 calc R U . . .
H1C H 0.638123 0.891700 0.534141 0.112 Uiso 1 1 calc R U . . .
C2 C 0.6384(9) 0.5917(8) 0.5815(2) 0.063(4) Uani 1 1 d D U . . .
H2A H 0.422397 0.456727 0.571345 0.076 Uiso 1 1 calc R U . . .
H2B H 0.782860 0.471420 0.588202 0.076 Uiso 1 1 calc R U . . .
C11 C -0.1419(12) 0.7158(9) 0.9527(3) 0.084(5) Uani 1 1 d D U . . .
H11A H -0.289279 0.831777 0.946611 0.126 Uiso 1 1 calc R U . . .
H11B H 0.073257 0.846119 0.962889 0.126 Uiso 1 1 calc R U . . .
H11C H -0.234253 0.582636 0.975783 0.126 Uiso 1 1 calc R U . . .

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
C6 0.065(2) 0.0488(15) 0.042(12) -0.002(4) -0.003(4) 0.0144(13)
C4 0.071(2) 0.0489(17) 0.051(13) -0.005(3) 0.000(4) 0.0151(14)
C8 0.067(2) 0.0510(16) 0.049(13) 0.002(3) 0.016(4) 0.0136(13)
C3 0.067(2) 0.0495(16) 0.047(13) -0.002(4) -0.001(5) 0.0155(14)
C9 0.073(2) 0.0569(17) 0.040(13) 0.006(4) 0.009(5) 0.0159(15)
C10 0.086(3) 0.075(2) 0.048(14) 0.009(4) 0.020(5) 0.0253(19)
C7 0.066(2) 0.0485(16) 0.041(12) 0.002(3) 0.005(4) 0.0150(13)
C5 0.065(2) 0.0480(16) 0.046(13) -0.003(4) 0.006(5) 0.0139(14)
C1 0.091(2) 0.079(2) 0.052(15) 0.003(4) 0.017(5) 0.0231(16)
C2 0.076(2) 0.0600(19) 0.051(14) -0.001(4) -0.003(5) 0.0166(15)
C11 0.113(3) 0.115(3) 0.034(14) 0.025(5) 0.019(7) 0.047(2)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.506(5) . ?
C6 C5 1.508(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.512(5) . ?
C4 C5 1.508(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.505(5) . ?
C8 C7 1.510(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.516(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.510(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.514(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C2 1.519(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H6A C6 H6B 107.5 . . ?
C7 C6 H6A 108.6 . . ?
C7 C6 H6B 108.6 . . ?
C7 C6 C5 114.8(3) . . ?
C5 C6 H6A 108.6 . . ?
C5 C6 H6B 108.6 . . ?
H4A C4 H4B 107.5 . . ?
C3 C4 H4A 108.4 . . ?
C3 C4 H4B 108.4 . . ?
C5 C4 H4A 108.4 . . ?
C5 C4 H4B 108.4 . . ?
C5 C4 C3 115.3(3) . . ?
H8A C8 H8B 107.6 . . ?
C9 C8 H8A 108.7 . . ?
C9 C8 H8B 108.7 . . ?
C9 C8 C7 114.4(3) . . ?
C7 C8 H8A 108.7 . . ?
C7 C8 H8B 108.7 . . ?
C4 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
C4 C3 C2 115.7(3) . . ?
H3A C3 H3B 107.4 . . ?
C2 C3 H3A 108.4 . . ?
C2 C3 H3B 108.4 . . ?
C8 C9 H9A 108.6 . . ?
C8 C9 H9B 108.6 . . ?
C8 C9 C10 114.6(3) . . ?
H9A C9 H9B 107.6 . . ?
C10 C9 H9A 108.6 . . ?
C10 C9 H9B 108.6 . . ?
C9 C10 H10A 108.6 . . ?
C9 C10 H10B 108.6 . . ?
C9 C10 C11 114.5(4) . . ?
H10A C10 H10B 107.6 . . ?
C11 C10 H10A 108.6 . . ?
C11 C10 H10B 108.6 . . ?
C6 C7 C8 115.0(3) . . ?
C6 C7 H7A 108.5 . . ?
C6 C7 H7B 108.5 . . ?
C8 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C6 C5 C4 115.4(3) . . ?
C6 C5 H5A 108.4 . . ?
C6 C5 H5B 108.4 . . ?
C4 C5 H5A 108.4 . . ?
C4 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C3 C2 C1 115.4(3) . . ?
C3 C2 H2A 108.4 . . ?
C3 C2 H2B 108.4 . . ?
C1 C2 H2A 108.4 . . ?
C1 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

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
C4 C3 C2 C1 -179.1(3) . . . . ?
C8 C9 C10 C11 179.4(4) . . . . ?
C3 C4 C5 C6 -179.7(3) . . . . ?
C9 C8 C7 C6 179.8(3) . . . . ?
C7 C6 C5 C4 179.8(3) . . . . ?
C7 C8 C9 C10 -179.4(3) . . . . ?
C5 C6 C7 C8 -179.8(3) . . . . ?
C5 C4 C3 C2 -179.6(3) . . . . ?

_shelx_res_file                  
;
TITL 0003_0001_a.res in P-1
    undecane.res
    created by SHELXL-2017/1 at 16:52:27 on 12-Jul-2023
REM Old TITL 0003_0001 in P-1
REM SHELXT solution in P-1: R1 0.284, Rweak 0.002, Alpha 0.131
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C11
CELL 0.41 4.180848 4.711303 29.529974 93.6092 90.4121 107.2737
ZERR 2 0.000483 0.000349 0.019758 0.019 0.0225 0.0086
LATT 1
SFAC C H
DISP C -0.0011 0.0005 5.0796
DISP H 0 0 0.5971
UNIT 22 48
DELU C1 C2 C3 C4 C5 C6 C7 C8 C9 C10 C11
ISOR 0.01 0.02 C11
SADI C1 C2 C2 C3
SADI C9 C10 C10 C11
SADI C3 C4 C4 C5
SADI C5 C6 C6 C7
SADI C7 C8 C8 C9
SADI C9 C8 C8 C7
SADI C7 C6 C7 C8
SADI C10 C9 C9 C8
SADI C5 C6 C5 C4
SADI C3 C4 C2 C3
DFIX 1.52 0.005 C11 C10 C9 C10 C9 C8 C8 C7 C7 C6 C6 C5 C5 C4 C4 C3 C3 C2 C2 C1

L.S. 4 0 0
PLAN  6
SIZE 0.12 0.22 0.02
TEMP 21.85
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta
SHEL 0.8 1000
OMIT -4 -1 6
REM <olex2.extras>
REM <HklSrc "%.\\undecane.hkl">
REM </olex2.extras>

WGHT    0.111200
FVAR      15.95135
C6    1    0.260640    0.557830    0.745850    11.00000    0.06487    0.04884 =
         0.04200   -0.00179   -0.00327    0.01436
AFIX  23
H6A   2    0.045131    0.419585    0.736254    11.00000   -1.20000
H6B   2    0.408819    0.441190    0.752688    11.00000   -1.20000
AFIX   0
C4    1    0.448944    0.573896    0.663888    11.00000    0.07078    0.04892 =
         0.05081   -0.00542   -0.00006    0.01506
AFIX  23
H4A   2    0.233964    0.435730    0.654053    11.00000   -1.20000
H4B   2    0.596829    0.456997    0.670734    11.00000   -1.20000
AFIX   0
C8    1    0.075955    0.545278    0.827763    11.00000    0.06747    0.05101 =
         0.04858    0.00232    0.01594    0.01361
AFIX  23
H8A   2   -0.140121    0.407167    0.818378    11.00000   -1.20000
H8B   2    0.224040    0.428623    0.834638    11.00000   -1.20000
AFIX   0
C3    1    0.591487    0.761930    0.624956    11.00000    0.06669    0.04945 =
         0.04668   -0.00214   -0.00144    0.01547
AFIX  23
H3A   2    0.806955    0.899292    0.634783    11.00000   -1.20000
H3B   2    0.444290    0.879819    0.618296    11.00000   -1.20000
AFIX   0
C9    1    0.033499    0.722126    0.870342    11.00000    0.07263    0.05695 =
         0.04014    0.00646    0.00868    0.01589
AFIX  23
H9A   2   -0.116263    0.837285    0.863503    11.00000   -1.20000
H9B   2    0.249200    0.861696    0.879514    11.00000   -1.20000
AFIX   0
C10   1   -0.102901    0.537145    0.909738    11.00000    0.08613    0.07497 =
         0.04822    0.00898    0.01983    0.02533
AFIX  23
H10A  2    0.045510    0.420334    0.916375    11.00000   -1.20000
H10B  2   -0.319781    0.399108    0.900694    11.00000   -1.20000
AFIX   0
C7    1    0.215644    0.731674    0.788630    11.00000    0.06621    0.04845 =
         0.04138    0.00170    0.00492    0.01500
AFIX  23
H7A   2    0.067030    0.847894    0.781785    11.00000   -1.20000
H7B   2    0.431074    0.870378    0.798145    11.00000   -1.20000
AFIX   0
C5    1    0.401086    0.744868    0.706919    11.00000    0.06542    0.04802 =
         0.04618   -0.00287    0.00554    0.01387
AFIX  23
H5A   2    0.615858    0.883800    0.716653    11.00000   -1.20000
H5B   2    0.252284    0.860960    0.700097    11.00000   -1.20000
AFIX   0
C1    1    0.786771    0.782178    0.542738    11.00000    0.09110    0.07873 =
         0.05200    0.00283    0.01740    0.02309
AFIX 137
H1A   2    0.816059    0.656339    0.517242    11.00000   -1.50000
H1B   2    0.999874    0.918853    0.552348    11.00000   -1.50000
H1C   2    0.638123    0.891700    0.534141    11.00000   -1.50000
AFIX   0
C2    1    0.638436    0.591723    0.581481    11.00000    0.07593    0.06005 =
         0.05118   -0.00082   -0.00257    0.01660
AFIX  23
H2A   2    0.422397    0.456727    0.571345    11.00000   -1.20000
H2B   2    0.782860    0.471420    0.588202    11.00000   -1.20000
AFIX   0
C11   1   -0.141859    0.715765    0.952685    11.00000    0.11347    0.11497 =
         0.03438    0.02543    0.01875    0.04662
AFIX 137
H11A  2   -0.289279    0.831777    0.946611    11.00000   -1.50000
H11B  2    0.073257    0.846119    0.962889    11.00000   -1.50000
H11C  2   -0.234253    0.582636    0.975783    11.00000   -1.50000
AFIX   0
HKLF 4




REM  0003_0001_a.res in P-1
REM R1 =  0.0539 for     253 Fo > 4sig(Fo)  and  0.1045 for all     586 data
REM    102 parameters refined using     80 restraints

END

WGHT      0.1112      0.0000

REM Highest difference peak  0.072,  deepest hole -0.070,  1-sigma level  0.023
Q1    1   0.0775  0.4720  0.6632  11.00000  0.05    0.07
Q2    1   0.2473  0.5102  0.6039  11.00000  0.05    0.07
Q3    1   0.0251  0.2956  0.7358  11.00000  0.05    0.06
Q4    1   0.5692  0.4770  0.4828  11.00000  0.05    0.06
Q5    1   0.3991  0.3319  0.7586  11.00000  0.05    0.06
Q6    1   0.2030  0.3091  0.8380  11.00000  0.05    0.06
;
_shelx_res_checksum              27023
loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 1.00000000 0.00000000 0.00000000
omega rotation goniometer -1 . -0.00106000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761
phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta rotation goniometer -1 . 0.00200000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_exptl_crystal_mounting_method DAC
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.425
_oxdiff_exptl_absorpt_empirical_full_min 0.756
# start Validation Reply Form
_vrf_PLAT029_undecane            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.268 Why?  
RESPONSE: Sample was measured in diamond anvil cell, which severly limits
	accessible reciprocal space
;
_vrf_PLAT088_undecane            
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.75 Note  
RESPONSE: a few reflections from triclinic crystal enclosed in a
	diamond anvil cell
;
_vrf_PLAT049_undecane            
;
PROBLEM: Calculated Density Less Than 1.0 gcm-3 .........     0.9368 Check 
RESPONSE: It is a typical feature of alkane crystals
;
_vrf_PLAT911_undecane            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        743 Report
RESPONSE: geometry of diamond anvil cell limits the accesible portion of
	the Ewald sphere
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 
'in-situ recrystallization from melt at high pressure in diamond anvil cell'
