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_2002968
_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         'C3 H2 F3 N'
_chemical_formula_sum            'C3 H2 F3 N'
_chemical_formula_weight         109.06
_chemical_name_systematic
;
2,2,2-trifluoroethyl isocyanide
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.668(2)
_cell_length_b                   9.266(3)
_cell_length_c                   8.626(2)
_cell_measurement_temperature    163.0(10)
_cell_volume                     453.0(2)
_computing_cell_refinement
;
Siemens software
;
_computing_data_collection
;
Siemens software
;
_computing_data_reduction        'in-house program'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163.0(10)
_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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1856
_diffrn_reflns_theta_max         34.98
_diffrn_reflns_theta_min         3.23
_diffrn_standards_decay_%        58
_diffrn_standards_interval_time  90
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_meas      ?
_exptl_crystal_description
;
cylinder with diameter 0.5 mm
;
_exptl_crystal_F_000             216
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.143
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.2(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.008
_refine_ls_goodness_of_fit_obs   1.044
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_restrained_S_obs      1.044
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_obs          0.0329
_refine_ls_shift/esd_max         0.006
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
 calc w=1/[\s^2^(Fo^2^) +
 (0.0452P)^2^+0.0656P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_wR_factor_all         0.0976
_refine_ls_wR_factor_obs         0.0839
_reflns_number_observed          1092
_reflns_number_total             1556
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ca0001.cif
_cod_data_source_block           III
_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               2002968