Insight into trifluoromethylation – experimental electron density for Togni reagent I
Wang, R.; Kalf, I.; Englert, U.; RSC Advances 8 (2018) 34287–; doi:10.1039/C8RA07187J

data_7231619
_publ_section_title
;
 Insight into trifluoromethylation -- experimental electron density for
 Togni reagent I
;
_journal_issue                   60
_journal_name_full               'RSC Advances'
_journal_page_first              34287
_journal_paper_doi               10.1039/C8RA07187J
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C10 H10 F3 I O'
_chemical_formula_sum            'C10 H10 F3 I O'
_chemical_formula_weight         330.08
_chemical_name_common            'compound 1, Togni reagent I'
_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
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             '14-Aug-08 T13:19:25-00:00'
_audit_creation_method           'XD routine XDCIF'
_audit_update_record
;
2018-08-16 deposited with the CCDC.
2018-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.2446(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1507(5)
_cell_length_b                   9.0836(5)
_cell_length_c                   13.3668(7)
_cell_measurement_reflns_used    19792
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.80
_cell_measurement_theta_min      2.24
_cell_volume                     1109.28(10)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'Volkov et al, (2006)'
_computing_publication_material  'Volkov et al, (2006)'
_computing_structure_refinement  'Volkov et al, (2006)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 gonimeter with APEX CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         'Incoatec microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            151509
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         51.430
_diffrn_reflns_theta_min         2.630
_exptl_absorpt_coefficient_mu    2.899
_exptl_absorpt_correction_T_max  0.579
_exptl_absorpt_correction_T_min  0.322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_description       'translucent block'
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         12366
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.034
_refine_ls_R_factor_gt           0.019
_refine_ls_shift/su_max          0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;    calc w2 = q/[s^2^(Fo^2^) + (0.03 P)^2^ + 0.14 P + 0.00 + 0.00 sin(th)]
     where P = (0.3333 Fo^2^ + 0.6667 Fc^2^)
           q = 1.0
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.050
_reflns_number_gt                10687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra07187j2.cif
_cod_data_source_block           mm
_cod_database_code               7231619
_shelx_estimated_absorpt_t_min   0.422
_shelx_estimated_absorpt_t_max   0.780