Generation and Synthetic Application of Trifluoromethyl Diazomethane Utilizing Continuous Flow Technologies.
Pieber, Bartholomäus; Kappe, C. Oliver; Organic letters 18 (2016) 1076–; doi:10.1021/acs.orglett.6b00194

data_1542702
_publ_section_title
;
 Generation and Synthetic Application of Trifluoromethyl Diazomethane
 Utilizing Continuous Flow Technologies.
;
_journal_issue                   5
_journal_name_full               'Organic letters'
_journal_page_first              1076
_journal_paper_doi               10.1021/acs.orglett.6b00194
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C10 H6 F3 N3 O'
_chemical_formula_sum            'C10 H6 F3 N3 O'
_chemical_formula_weight         241.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-19 # Formatted by publCIF

;
_cell_angle_alpha                99.340(2)
_cell_angle_beta                 92.3230(10)
_cell_angle_gamma                91.732(2)
_cell_formula_units_Z            2
_cell_length_a                   7.0244(3)
_cell_length_b                   7.2782(3)
_cell_length_c                   10.3940(4)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.24
_cell_measurement_theta_min      2.84
_cell_volume                     523.55(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24321
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.243
_diffrn_reflns_theta_min         2.838
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       block
_exptl_crystal_F_000             244
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0606P)^2^+0.1515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1170
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3260
_reflns_number_total             3979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b00194_si_002.cif
_cod_data_source_block           AT515_a
_cod_database_code               1542702
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.989
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              69261
_shelx_hkl_checksum              14554