Low-temperature and high-pressure polymorphs of isopropyl alcohol
Ridout, Joe; Probert, Michael R.; CrystEngComm 16 (2014) 7397–; doi:10.1039/C4CE01012D

data_7216777
_publ_section_title
;
 Low-temperature and high-pressure polymorphs of isopropyl alcohol
;
_journal_issue                   32
_journal_name_full               CrystEngComm
_journal_page_first              7397
_journal_paper_doi               10.1039/C4CE01012D
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C3 H8 O'
_chemical_formula_sum            'C3 H8 O'
_chemical_formula_weight         60.09
_chemical_name_systematic        Isopropanol
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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
_audit_creation_date             2014-04-01
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.03.20 svn.r2918 for OlexSys, GUI svn.r4813)
;
_cell_angle_alpha                90
_cell_angle_beta                 118.243(8)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   8.7267(18)
_cell_length_b                   21.838(6)
_cell_length_c                   8.408(3)
_cell_measurement_reflns_used    85
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      14.94
_cell_measurement_theta_min      3.73
_cell_volume                     1411.6(7)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.290
_diffrn_measured_fraction_theta_max 0.603
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  IuS_Ag_high_pressure
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_collimation    'Multilayer mirrors'
_diffrn_radiation_monochromator  'Bruker Helios multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0877
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 0.290
_diffrn_reflns_Laue_measured_fraction_max 0.603
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            6526
_diffrn_reflns_point_group_measured_fraction_full 0.290
_diffrn_reflns_point_group_measured_fraction_max 0.603
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         15.340
_diffrn_reflns_theta_min         2.216
_diffrn_source                   'Microfocus sealed tube'
_diffrn_source_target            Ag
_diffrn_source_type              'Incoatec IuS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.052
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.4837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0990 before and 0.0593 after correction.
The Ratio of minimum to maximum transmission is 0.6501.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_recrystallization_method
'Crystallised at high-pressure in a diamond anvil cell'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.145
_refine_diff_density_min         -0.143
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         743
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0585
_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/[\s^2^(Fo^2^)+(0.0476P)^2^+2.4683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                503
_reflns_number_total             743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce01012d1.cif
_cod_data_source_block           test1
_cod_depositor_comments
;Adding full bibliography for 7216777--7216778.cif.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1411.5(6)
_cod_database_code               7216777
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.987
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
C16A \\sim C11A \\sim C14A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C16) = Uanis(C16A)
Uanis(C14) = Uanis(C14A)
Uanis(C11) = Uanis(C11A)
3. Others
 Sof(C16A)=Sof(H16d)=Sof(H16e)=Sof(H16f)=Sof(C14A)=Sof(H14A)=Sof(C11A)=
 Sof(H11d)=Sof(H11e)=Sof(H11f)=1-FVAR(1)
 Sof(C11)=Sof(H11a)=Sof(H11b)=Sof(H11c)=Sof(C14)=Sof(H14)=Sof(C16)=Sof(H16a)=
 Sof(H16b)=Sof(H16c)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C6(H6), C14(H14), C17(H17), C2(H2a), C14A(H14A)
4.b Tetrahedral OH refined with riding coordinates:
 O3(H3)
4.c Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C10(H10a,H10b,H10c),
 C11(H11a,H11b,H11c), C16(H16a,H16b,H16c), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c),
 C16A(H16d,H16e,H16f), C11A(H11d,H11e,H11f)
4.d Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4), O1(H1)
;
_shelx_res_checksum              73606