Polymorphism Arising from Differing Rates of Compression of Liquids
Ridout, Joe; Price, Louise S.; Howard, Judith A. K.; Probert, Michael R.; Crystal Growth & Design 14 (2014) 3384–; doi:10.1021/cg500331u

data_4511275
_publ_section_title
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 Polymorphism Arising from Differing Rates of Compression of Liquids
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_journal_issue                   7
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3384
_journal_paper_doi               10.1021/cg500331u
_journal_volume                  14
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C8 H5 F'
_chemical_formula_sum            'C8 H5 F'
_chemical_formula_weight         120.12
_chemical_name_systematic        2-fluorophenylacetylene
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-03-04
_audit_creation_method
;
  Olex2 1.2-alpha
  (compiled 2013.04.25 svn.r2679, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.467(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   3.9343(7)
_cell_length_b                   5.9336(10)
_cell_length_c                   12.962(4)
_cell_measurement_reflns_used    528
_cell_measurement_temperature    293
_cell_measurement_theta_max      10.323
_cell_measurement_theta_min      3.51
_cell_volume                     299.29(12)
_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    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_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 0.414
_diffrn_measured_fraction_theta_max 0.414
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0184
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            686
_diffrn_reflns_theta_full        17.99
_diffrn_reflns_theta_max         17.99
_diffrn_reflns_theta_min         2.99
_diffrn_source                   'Microfocus sealed tube'
_diffrn_source_target            Ag
_diffrn_source_type              'Incoatec IuS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_T_max  0.7442
_exptl_absorpt_correction_T_min  0.6049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0483 before and 0.0283 after correction.
The Ratio of minimum to maximum transmission is 0.8128.
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    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cylinder
_exptl_crystal_F_000             124
_exptl_crystal_recrystallization_method
' Crystallised at high-pressure in a diamond anvil cell with a high-rate of compression'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_exptl_crystal_size_rad          0.25
_refine_diff_density_max         0.078
_refine_diff_density_min         -0.092
_refine_diff_density_rms         0.022
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         353
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0346
_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/[\s^2^(Fo^2^)+(0.0264P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0630
_reflns_number_gt                271
_reflns_number_total             353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg500331u_si_005.cif
_cod_data_source_block           pmorph3
_cod_depositor_comments
'Adding full bibliography for 4511275--4511277.cif.'
_cod_original_cell_volume        299.28(11)
_cod_database_code               4511275
_olex2_refinement_description
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1. Others
 Fixed Uiso: H5(0.078) H2(0.067) H3(0.085) H6(0.08) H1(0.087) H4(0.087)
 Fixed X: H5(-0.0958) H2(0.4972) H3(0.3584) H6(0.0527) H1(0.5095) H4(0.0747)
 Fixed Y: H5(-0.0077) H2(0.6388) H3(0.401) H6(0.2281) H1(0.8533) H4(0.0692)
 Fixed Z: H5(0.2481) H2(0.3436) H3(0.47) H6(0.1192) H1(0.034) H4(0.4169)
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