#------------------------------------------------------------------------------
#$Date: 2020-12-20 03:21:21 +0100 (dom 20 de dic de 2020) $
#$Revision: 260032 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/19/7241928.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7241928
loop_
_publ_author_name
'Liu, X.'
'Pulham, C. R.'
_publ_section_title
;
 Pressure-induced phase separation of miscible liquids:
 1 : 1 n-pentane/iso-pentane
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              8251
_journal_page_last               8255
_journal_paper_doi               10.1039/D0CE01335H
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'C5 H12'
_chemical_formula_sum            'C5 H12'
_chemical_formula_weight         72.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc260y9h
_audit_creation_date             2020-09-01
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-09-01 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.7996(7)
_cell_length_b                   8.2477(13)
_cell_length_c                   14.205(4)
_cell_measurement_reflns_used    864
_cell_measurement_temperature    275.2
_cell_measurement_theta_max      24.79
_cell_measurement_theta_min      4.94
_cell_volume                     445.16(17)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      275.2
_diffrn_measured_fraction_theta_full 0.586
_diffrn_measured_fraction_theta_max 0.587
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.586
_diffrn_reflns_Laue_measured_fraction_max 0.587
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2022
_diffrn_reflns_point_group_measured_fraction_full 0.586
_diffrn_reflns_point_group_measured_fraction_max 0.587
_diffrn_reflns_theta_full        24.958
_diffrn_reflns_theta_max         24.958
_diffrn_reflns_theta_min         4.943
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.058
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_description       plate
_exptl_crystal_F_000             168
_exptl_crystal_preparation       'at 3.3 GPa'
_refine_diff_density_max         0.118
_refine_diff_density_min         -0.128
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         233
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0437
_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)+(0.0703P)²+0.0577P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1270
_reflns_Friedel_coverage         0.000
_reflns_number_gt                186
_reflns_number_total             233
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01335h2.cif
_cod_data_source_block           pentane_pbcn
_cod_database_code               7241928
_shelx_shelxl_version_number     2018/3
_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.
;
_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. Others
 Fixed Sof: H00A(0.5) H00B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C001(H00A,H00B), C002(H00D,H00C)
3.b Idealised Me refined as rotating group:
 C003(H00E,H00F,H00G)
;
_shelx_res_file
;
TITL pentane_pbcn_a.res in Pbcn
    pentane_pbcn.res
    created by SHELXL-2018/3 at 17:02:30 on 02-May-2020
REM Old TITL PENTANE_PBCN in Pbcn
REM SHELXT solution in Pbcn: R1 0.152, Rweak 0.011, Alpha 0.034
REM <I/s> 1.204 for 45 systematic absences, Orientation as input
REM Formula found by SHELXT: C5
CELL 0.71073 3.7996 8.2477 14.2052 90 90 90
ZERR 4 0.0007 0.0013 0.0041 0 0 0
LATT 1
SYMM 0.5-X,0.5-Y,0.5+Z
SYMM -X,+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H
UNIT 20 48

L.S. 10
PLAN  20
TEMP 2.05
CONF
BOND
list 4
fmap 2 53
MORE -1
ACTA
BOND $H
OMIT 1 0 6
OMIT 3 2 3
OMIT 0 4 0
OMIT 1 3 3
OMIT 0 4 1
REM <olex2.extras>
REM <HklSrc "%.\\PENTANE_PBCN.hkl">
REM </olex2.extras>

WGHT    0.070300    0.057700
FVAR       2.07609
C001  1    0.500000    0.629842    0.750000    10.50000    0.03022    0.02471 =
         0.02899    0.00000    0.00007    0.00000
AFIX  23
H00A  2    0.303166    0.699292    0.733725    10.50000   -1.20000
H00B  2    0.696832    0.699294    0.766275    10.50000   -1.20000
AFIX   0
C002  1    0.598488    0.530636    0.664781    11.00000    0.03472    0.02707 =
         0.02870   -0.00231   -0.00054    0.00025
AFIX  23
H00D  2    0.787868    0.457393    0.681764    11.00000   -1.20000
H00C  2    0.397746    0.465202    0.646442    11.00000   -1.20000
AFIX   0
C003  1    0.713183    0.630893    0.581621    11.00000    0.03779    0.03672 =
         0.03244   -0.00260   -0.00002   -0.00109
AFIX 137
H00E  2    0.758998    0.560974    0.529000    11.00000   -1.50000
H00F  2    0.923421    0.689426    0.597429    11.00000   -1.50000
H00G  2    0.530226    0.706172    0.565436    11.00000   -1.50000
AFIX   0
HKLF 4




REM  pentane_pbcn_a.res in Pbcn
REM wR2 = 0.1270, GooF = S = 1.190, Restrained GooF = 1.190 for all data
REM R1 = 0.0437 for 186 Fo > 4sig(Fo) and 0.0575 for all 233 data
REM 25 parameters refined using 0 restraints

END

WGHT      0.0703      0.0577

REM Highest difference peak  0.118,  deepest hole -0.128,  1-sigma level  0.035
Q1    1   0.0000  0.6229  0.7500  10.50000  0.05    0.12
Q2    1   0.4311  0.8709  0.5801  11.00000  0.05    0.11
Q3    1   1.1831  0.6383  0.5870  11.00000  0.05    0.10
Q4    1   0.3996  0.6569  0.5277  11.00000  0.05    0.09
Q5    1   0.4641  0.5818  0.5406  11.00000  0.05    0.09
Q6    1   0.3511  0.5256  0.5772  11.00000  0.05    0.09
Q7    1   0.1925  0.6608  0.6980  11.00000  0.05    0.09
Q8    1   0.5809  0.5795  0.5014  11.00000  0.05    0.09
Q9    1   0.5000  0.7599  0.7500  10.50000  0.05    0.09
Q10   1   0.6154  0.4127  0.6621  11.00000  0.05    0.09
Q11   1   0.9948  0.7736  0.6836  11.00000  0.05    0.09
Q12   1   0.8259  0.7508  0.6356  11.00000  0.05    0.08
Q13   1   0.5289  0.5729  0.5208  11.00000  0.05    0.08
Q14   1   0.2986  0.7208  0.6822  11.00000  0.05    0.08
Q15   1   0.2967  0.4189  0.6419  11.00000  0.05    0.08
Q16   1   0.6800  0.3782  0.6740  11.00000  0.05    0.08
Q17   1   0.6602  0.7503  0.8071  11.00000  0.05    0.08
Q18   1   1.0051  0.5534  0.5792  11.00000  0.05    0.08
Q19   1   0.8255  0.4532  0.7225  11.00000  0.05    0.08
Q20   1   0.8394  0.3793  0.7517  11.00000  0.05    0.07
;
_shelx_res_checksum              66241
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'
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
C001 C 0.500000 0.6298(2) 0.750000 0.0280(11) Uani 1 2 d S T P . .
H00A H 0.303166 0.699292 0.733725 0.034 Uiso 0.5 1 calc R U P . .
H00B H 0.696832 0.699294 0.766275 0.034 Uiso 0.5 1 calc R U P . .
C002 C 0.5985(5) 0.53064(19) 0.6648(2) 0.0302(9) Uani 1 1 d . . . . .
H00D H 0.787868 0.457393 0.681764 0.036 Uiso 1 1 calc R U . . .
H00C H 0.397746 0.465202 0.646442 0.036 Uiso 1 1 calc R U . . .
C003 C 0.7132(6) 0.6309(2) 0.5816(2) 0.0356(10) Uani 1 1 d . . . . .
H00E H 0.758998 0.560974 0.529000 0.053 Uiso 1 1 calc R U . . .
H00F H 0.923421 0.689426 0.597429 0.053 Uiso 1 1 calc R U . . .
H00G H 0.530226 0.706172 0.565436 0.053 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
C001 0.030(2) 0.0247(11) 0.029(4) 0.000 0.0001(14) 0.000
C002 0.0347(17) 0.0271(9) 0.029(3) -0.0023(10) -0.0005(9) 0.0003(7)
C003 0.0378(18) 0.0367(10) 0.032(3) -0.0026(11) 0.0000(10) -0.0011(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
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
H00A C001 H00B 107.6 . . ?
C002 C001 H00A 108.7 3_656 . ?
C002 C001 H00A 108.7 . . ?
C002 C001 H00B 108.7 3_656 . ?
C002 C001 H00B 108.7 . . ?
C002 C001 C002 114.3(2) . 3_656 ?
C001 C002 H00D 108.8 . . ?
C001 C002 H00C 108.8 . . ?
H00D C002 H00C 107.7 . . ?
C003 C002 C001 113.79(15) . . ?
C003 C002 H00D 108.8 . . ?
C003 C002 H00C 108.8 . . ?
C002 C003 H00E 109.5 . . ?
C002 C003 H00F 109.5 . . ?
C002 C003 H00G 109.5 . . ?
H00E C003 H00F 109.5 . . ?
H00E C003 H00G 109.5 . . ?
H00F C003 H00G 109.5 . . ?
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
C001 H00A 0.9700 . ?
C001 H00B 0.9700 . ?
C001 C002 1.508(3) . ?
C001 C002 1.508(3) 3_656 ?
C002 H00D 0.9700 . ?
C002 H00C 0.9700 . ?
C002 C003 1.506(3) . ?
C003 H00E 0.9600 . ?
C003 H00F 0.9600 . ?
C003 H00G 0.9600 . ?
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
C002 C001 C002 C003 -177.2(2) 3_656 . . . ?
