High-Pressure and Low-Temperature Polymorphism in C–H···F–C Hydrogen Bonded Monofluorotoluenes
Ridout, Joe; Probert, Michael R.; Crystal Growth & Design 13 (2013) 1943–; doi:10.1021/cg301773h

data_4507558
_publ_section_title
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 High-Pressure and Low-Temperature Polymorphism in
 C--H&#x00B7;&#x00B7;&#x00B7;F--C Hydrogen Bonded Monofluorotoluenes
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_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1943
_journal_paper_doi               10.1021/cg301773h
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         'C7 H7 F'
_chemical_formula_sum            'C7 H7 F'
_chemical_formula_weight         110.13
_chemical_name_systematic        3-fluorotoluene
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-11-19
_audit_creation_method
;
  Olex2 1.2-alpha
  (compiled 2012.02.07 svn.r2199, GUI svn.r4069)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.67(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.223(9)
_cell_length_b                   7.623(10)
_cell_length_c                   12.098(16)
_cell_measurement_reflns_used    719
_cell_measurement_temperature    179
_cell_measurement_theta_max      24.30
_cell_measurement_theta_min      3.19
_cell_volume                     641.4(14)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2001)'
_computing_data_collection       'SMART v5.049 (Bruker, 1999)'
_computing_data_reduction        'SAINT V7.68A (Bruker, 2001)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      179
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.710
_diffrn_measured_fraction_theta_max 0.710
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1033
_diffrn_reflns_theta_full        24.35
_diffrn_reflns_theta_max         24.35
_diffrn_reflns_theta_min         3.19
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.1078 before and 0.0349 after correction.
The Ratio of minimum to maximum transmission is 0.6691.
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    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             232
_exptl_crystal_recrystallization_method 'Cryo-crystallised in a Lindemann tube.'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.155
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0960P)^2^+0.0998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1520
_reflns_number_gt                631
_reflns_number_total             747
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg301773h_si_005.cif
_cod_data_source_block           final
_cod_original_cell_volume        641.4(15)
_cod_database_code               4507558
_olex2_refinement_description
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1. Others
 Fixed Uiso: H1(0.057) H2(0.065) H3(0.07) H4(0.063) H6(0.103) H5(0.103)
 H7(0.103)
 Fixed X: H1(0.2578) H2(-0.2244) H3(-0.2326) H4(0) H6(0.3816) H5(0.2515)
 H7(0.3961)
 Fixed Y: H1(0.0071) H2(0.2725) H3(0.3926) H4(0.3189) H6(0.2141) H5(0.0633)
 H7(0.0247)
 Fixed Z: H1(0.2504) H2(0.2535) H3(0.0749) H4(-0.0154) H6(0.0414) H5(-0.0262)
 H7(0.0935)
;