#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/18/1511808.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_1511808
loop_
_publ_author_name
'Podsiadło, Marcin'
'Olejniczak, Anna'
'Katrusiak, Andrzej'
_publ_section_title
;
 Why Propane?
;
_journal_issue                   9
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              4759
_journal_paper_doi               10.1021/jp311747m
_journal_volume                  117
_journal_year                    2013
_chemical_formula_moiety         'C4 H10'
_chemical_formula_sum            'C4 H10'
_chemical_formula_weight         58.12
_chemical_melting_point          135
_chemical_name_common            butane
_chemical_name_systematic
; 
butane phase II 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.78(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.416(5)
_cell_length_b                   4.893(4)
_cell_length_c                   7.294(7)
_cell_measurement_reflns_used    184
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.61
_cell_measurement_theta_min      5.07
_cell_volume                     186.9(3)
_computing_cell_refinement       'CrysAlisRED (Oxford Diffraction, 2004)'
_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2004)'
_computing_data_reduction
'CrysAlisRED (Oxford Diffraction, 2004); REDSHABS (Katrusiak, A.  2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  'SHELXL--97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL--97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS--97 (Sheldrick, 1997)'
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         2500000
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.308
_diffrn_measured_fraction_theta_max 0.308
_diffrn_measurement_device_type  'KM-4 CCD'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            755
_diffrn_reflns_theta_full        26.61
_diffrn_reflns_theta_max         26.61
_diffrn_reflns_theta_min         5.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.056
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Correction for absorption of the diamond-anvil cell and the sample 
 were made using program REDSHABS (Katrusiak, A. (2003) REDSHABS. Adam
 Mickiewicz University Poznań; Katrusiak, A. (2004) Z. Kristallogr.
 219, 461-467).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.033
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cylinder
_exptl_crystal_F_000             68
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.081
_refine_diff_density_min         -0.060
_refine_diff_density_rms         0.020
_refine_ls_extinction_coef       0.08(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.259
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     20
_refine_ls_number_reflns         120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.259
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0445P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                86
_reflns_number_total             120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp311747m_si_002.cif
_cod_data_source_block           3pow_2.50GPa
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1511808
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.1333(8) -0.0151(8) 0.0589(6) 0.0273(17) Uani 1 1 d .
H2 H 0.2247 -0.1380 -0.0049 0.033 Uiso 1 1 calc R
H1 H 0.1298 -0.0979 0.1790 0.033 Uiso 1 1 calc R
C2 C 0.2782(9) 0.2548(10) 0.0973(6) 0.037(2) Uani 1 1 d .
H3 H 0.4453 0.2231 0.1786 0.055 Uiso 1 1 calc R
H5 H 0.1870 0.3794 0.1579 0.055 Uiso 1 1 calc R
H4 H 0.2933 0.3319 -0.0204 0.055 Uiso 1 1 calc R
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 0.018(6) 0.035(8) 0.025(4) 0.004(3) -0.001(4) -0.003(2)
C2 0.038(8) 0.038(7) 0.032(5) 0.000(2) 0.005(6) -0.005(3)
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
C1 C1 C2 113.5(5) 3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C1 1.487(9) 3
C1 C2 1.525(5) .
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_calc
_refln_F_squared_meas
_refln_F_squared_sigma
_refln_observed_status
1 1 0 287.81 300.85 2.14 o
2 1 0 59.02 60.09 0.95 o
1 2 0 131.45 125.36 0.94 o
2 2 0 46.36 46.33 0.95 o
3 2 0 73.00 73.42 1.68 o
2 3 0 0.02 1.41 0.90 o
3 3 0 7.49 7.64 0.99 o
4 3 0 2.59 5.01 1.34 o
4 4 0 1.23 2.61 1.19 o
-2 1 1 16.53 15.49 0.81 o
-1 1 1 237.39 252.72 4.63 o
0 1 1 291.01 282.57 3.02 o
1 1 1 37.00 37.88 1.08 o
-4 2 1 0.01 2.00 1.21 o
-3 2 1 0.26 1.07 0.43 o
-2 2 1 14.69 14.27 1.36 o
1 2 1 63.12 63.53 3.70 o
2 2 1 1.52 1.37 0.46 o
3 2 1 2.87 0.75 3.17 o
-4 3 1 14.39 14.23 1.30 o
-3 3 1 7.99 8.19 1.03 o
2 3 1 11.18 11.92 1.28 o
3 3 1 15.10 15.90 1.37 o
-5 4 1 1.31 4.84 1.48 o
3 4 1 0.50 1.89 1.13 o
4 4 1 1.19 2.60 1.37 o
-2 0 2 3.84 2.97 0.61 o
-1 0 2 1129.22 1113.50 22.29 o
-3 1 2 32.03 30.59 1.07 o
-2 1 2 42.58 47.40 1.02 o
0 1 2 208.51 198.53 2.43 o
1 1 2 0.55 0.90 0.37 o
-4 2 2 60.84 62.94 2.20 o
-3 2 2 3.86 3.69 0.53 o
-2 2 2 138.34 146.48 2.55 o
0 2 2 12.16 12.30 2.66 o
1 2 2 57.45 58.08 1.43 o
2 2 2 27.33 28.45 1.74 o
-5 3 2 3.65 3.97 2.98 o
-4 3 2 1.29 2.28 0.75 o
-3 3 2 6.07 4.80 2.18 o
1 3 2 7.21 6.55 0.65 o
2 3 2 12.22 11.32 1.06 o
3 3 2 0.00 0.20 1.69 o
-5 4 2 3.06 2.76 2.03 o
3 4 2 0.26 2.17 1.04 o
-4 1 3 7.07 7.40 2.90 o
-3 1 3 0.88 1.02 0.40 o
-2 1 3 39.03 37.49 0.71 o
-1 1 3 101.34 99.14 0.90 o
0 1 3 23.67 23.08 0.63 o
-4 2 3 0.14 1.34 0.70 o
-3 2 3 0.30 1.20 0.62 o
0 2 3 1.84 1.68 0.82 o
1 2 3 2.01 1.83 0.46 o
2 2 3 0.49 1.93 0.91 o
-5 3 3 8.56 7.74 2.31 o
-4 3 3 6.75 3.76 2.17 o
1 3 3 7.45 6.59 0.95 o
2 3 3 17.07 14.73 1.42 o
2 4 3 0.69 2.03 0.85 o
3 4 3 0.36 2.52 1.23 o
-3 0 4 4.57 5.54 1.77 o
-2 0 4 91.64 93.28 1.10 o
-1 0 4 121.90 126.87 4.05 o
-4 1 4 13.06 14.07 2.42 o
-3 1 4 2.13 1.83 0.64 o
-2 1 4 28.68 27.81 0.65 o
-1 1 4 42.70 42.22 1.93 o
0 1 4 10.82 11.49 0.72 o
-5 2 4 31.18 27.50 2.19 o
-4 2 4 0.62 1.81 0.91 o
-3 2 4 49.93 54.99 2.60 o
-1 2 4 0.14 0.81 0.58 o
0 2 4 25.13 26.27 0.91 o
1 2 4 2.34 0.66 2.70 o
-5 3 4 0.00 0.24 1.41 o
0 3 4 14.56 14.73 0.85 o
1 3 4 5.49 5.36 0.95 o
2 3 4 1.41 3.06 1.26 o
2 4 4 0.33 1.71 0.91 o
-4 1 5 0.14 1.38 0.82 o
-3 1 5 10.86 9.19 1.14 o
-2 1 5 28.59 29.22 1.95 o
-1 1 5 14.77 13.09 1.01 o
-5 2 5 0.00 2.02 1.47 o
-4 2 5 0.36 2.51 1.05 o
-1 2 5 0.14 1.51 0.72 o
0 2 5 0.08 1.80 0.60 o
0 3 5 2.97 2.61 1.03 o
1 3 5 12.30 11.65 1.33 o
1 4 5 0.89 1.98 1.25 o
2 4 5 0.05 2.06 1.28 o
-4 0 6 2.32 2.92 1.73 o
-3 0 6 16.16 12.13 1.80 o
-2 0 6 68.16 74.82 3.23 o
-5 1 6 5.70 8.86 5.24 o
-4 1 6 1.00 2.17 1.19 o
-3 1 6 13.23 8.99 2.49 o
-2 1 6 1.61 1.71 0.65 o
-1 1 6 13.99 10.54 1.86 o
-5 2 6 3.11 4.01 2.29 o
-2 2 6 0.05 1.62 1.08 o
-1 2 6 5.92 4.42 1.03 o
0 2 6 0.32 2.30 1.33 o
0 3 6 0.24 2.81 1.37 o
1 3 6 3.10 4.98 2.95 o
1 4 6 1.39 2.68 2.24 o
-5 1 7 0.00 3.91 1.63 o
-4 1 7 5.50 3.39 1.46 o
-3 1 7 11.87 14.87 1.13 o
-2 1 7 5.38 6.02 1.44 o
-2 2 7 0.23 1.19 0.95 o
-1 2 7 0.43 2.51 1.07 o
-1 3 7 0.77 2.64 1.54 o
0 3 7 6.69 7.78 2.73 o
-4 0 8 1.96 3.23 1.97 o
-3 1 8 0.91 2.40 1.38 o
-2 2 8 0.15 3.65 1.92 o
-1 3 8 0.54 1.75 2.21 o
