Low-temperature crystallization and structure determination of <i>N</i>-(trifluoromethyl)formamide, <i>N</i>-(2,2,2-trifluoroethyl)formamide and 2,2,2-trifluoroethyl isocyanide
Perpetuo, Genivaldo; Buschmann, Jürgen; Luger, Peter; Lentz, Dieter; Dreissig, D.; Acta Crystallographica Section B 55 (1999) 70–77; doi:10.1107/S0108768198006570

data_2002966
_publ_section_title
;
 Low-temperature crystallization and structure determination of
 <i>N</i>-(trifluoromethyl)formamide,
 <i>N</i>-(2,2,2-trifluoroethyl)formamide and 2,2,2-trifluoroethyl
 isocyanide
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              70
_journal_page_last               77
_journal_paper_doi               10.1107/S0108768198006570
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         'C2 H2 F3 N O'
_chemical_formula_sum            'C2 H2 F3 N O'
_chemical_formula_weight         113.05
_chemical_name_systematic
;
N-trifluoromethyl formamide
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.547(2)
_cell_length_b                   5.947(3)
_cell_length_c                   14.731(9)
_cell_measurement_temperature    143.0(10)
_cell_volume                     398.3(4)
_computing_cell_refinement
;
Siemens software
;
_computing_data_collection
;
Siemens software
;
_computing_data_reduction        'in-house program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143.0(10)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device
;
Siemens four circle diffractometer, N2 gas stream cooled
;
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  none
_diffrn_radiation_source         'fine-focus x-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71068
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2446
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.77
_diffrn_standards_decay_%        4
_diffrn_standards_interval_time  90
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_density_meas      ?
_exptl_crystal_description
;
cylinder with diameter 0.5 mm
;
_exptl_crystal_F_000             224
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.389
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -2.88(2.96)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.105
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1170
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.167
_refine_ls_restrained_S_obs      1.167
_refine_ls_R_factor_all          0.1230
_refine_ls_R_factor_obs          0.0696
_refine_ls_shift/esd_max         0.086
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w=1/[\s^2^(Fo^2^) +
 (0.0749P)^2^+0.5432P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_wR_factor_all         0.2259
_refine_ls_wR_factor_obs         0.1708
_reflns_number_gt                779
_reflns_number_total             1170
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ca0001.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'no' was replaced with
'none' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P21 21 21'
_cod_database_code               2002966