Aluminum–Catalyzed Tunable Halodefluorination of Trifluoromethyl- and Difluoroalkyl-Substituted Olefins
Liu, Zhong; Tu, Xian-Shuang; Guo, Le-Tao; Wang, Xiao-Chen; Chemical Science  (2020) –; doi:10.1039/D0SC03883K

data_1559239
_publ_section_title
;
 Aluminum--Catalyzed Tunable Halodefluorination of Trifluoromethyl- and
 Difluoroalkyl-Substituted Olefins
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03883K
_journal_year                    2020
_chemical_formula_sum            'C15 H11 Cl3'
_chemical_formula_weight         297.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-05-13 deposited with the CCDC.	2020-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                105.723(5)
_cell_angle_beta                 108.005(5)
_cell_angle_gamma                100.048(4)
_cell_formula_units_Z            8
_cell_length_a                   13.0257(7)
_cell_length_b                   13.3355(7)
_cell_length_c                   18.0392(9)
_cell_measurement_reflns_used    12015
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      31.0430
_cell_measurement_theta_min      2.3330
_cell_volume                     2752.0(3)
_computing_cell_refinement       crystalclear
_computing_data_collection       crystalclear
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'rigaku saturn'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
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_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21382
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.020
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_min         1.654
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.69505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.298
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         9633
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.0986
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1770P)^2^+9.2942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2926
_refine_ls_wR_factor_ref         0.3124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7399
_reflns_number_total             9633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03883k2.cif
_cod_data_source_block           r20191017b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

2022-06-10
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum        'C30 H22 Cl6'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     595.17
_cod_database_code               1559239
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.882
_shelx_estimated_absorpt_t_max   0.927
_shelx_res_checksum              85918