Crystal Structure of 2,8-Bis(trifluoromethyl)-4-vinylquinoline
GUILLON, Jean; DASSONVILLE-KLIMPT, Alexandra; MOREAU, Stéphane; LAUMAILLE, Pierre; MARCHIVIE, Mathieu; SONNET, Pascal; X-ray Structure Analysis Online 34 (2018) 15–; doi:10.2116/xraystruct.34.15

data_1551563
_publ_section_title
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 Crystal Structure of 2,8-Bis(trifluoromethyl)-4-vinylquinoline
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              15
_journal_paper_doi               10.2116/xraystruct.34.15
_journal_volume                  34
_journal_year                    2018
_chemical_formula_moiety         'C13 H7 F6 N'
_chemical_formula_sum            'C13 H7 F6 N'
_chemical_formula_weight         291.19
_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             2017-07-21
_audit_creation_method
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Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.50(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.678(2)
_cell_length_b                   17.492(7)
_cell_length_c                   8.286(4)
_cell_measurement_reflns_used    3773
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.025
_cell_measurement_theta_min      2.635
_cell_volume                     2396.6(15)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15792
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.635
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0864 before and 0.0589 after correction.
The Ratio of minimum to maximum transmission is 0.9156.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         4195
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.233
_refine_ls_R_factor_all          0.2051
_refine_ls_R_factor_gt           0.1043
_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^)+(0.0300P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1891
_refine_ls_wR_factor_ref         0.2207
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1895
_reflns_number_total             4195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            34_15_1.txt
_cod_data_source_block           vinyl-meflo
_cod_depositor_comments
;

2022-11-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
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_cod_original_cell_volume        2396.5(16)
_cod_original_formula_moiety     '2(C13 H7 F6 N)'
_cod_original_formula_sum        'C26 H14 F12 N2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     582.39
_cod_database_code               1551563
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
F9A \\sim F9B \\sim F7A \\sim F7B \\sim F8A \\sim F8B: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
F1B \\sim F1A \\sim F2B \\sim F2A \\sim F3B \\sim F3A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(F3B)=Sof(F1B)=Sof(F2B)=1-FVAR(1)
 Sof(F3A)=Sof(F1A)=Sof(F2A)=FVAR(1)
 Sof(F9B)=Sof(F7B)=Sof(F8B)=1-FVAR(2)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C16(H16), C3(H3), C10(H10), C24(H24), C22(H22), C21(H21), C11(H11),
 C8(H8), C9(H9)
5.b X=CH2 refined with riding coordinates:
 C25(H25A,H25B), C12(H12A,H12B)
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_olex2_submission_special_instructions 'No special instructions were received'