Generation of Hydrofluoronickelacycles from Trifluoroethylene and Ni(0): Ligand Effects on Regio-/Stereoselectivity and Reactivity.
Giffin, Kaitie A.; Pua, Lorraine A.; Piotrkowski, Sarah; Gabidullin, Bulat M.; Korobkov, Ilia; Hughes, Russell P.; Baker, R. Tom; Journal of the American Chemical Society 139 (2017) 4075–4086; doi:10.1021/jacs.6b12607

data_4125887
_publ_section_title
;
 Generation of Hydrofluoronickelacycles from Trifluoroethylene and Ni(0):
 Ligand Effects on Regio-/Stereoselectivity and Reactivity.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4075
_journal_page_last               4086
_journal_paper_doi               10.1021/jacs.6b12607
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C20 H24 B2 F10 P2'
_chemical_formula_weight         537.95
_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_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 105.557(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.886(3)
_cell_length_b                   14.270(6)
_cell_length_c                   12.665(6)
_cell_measurement_reflns_used    2481
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.20
_cell_volume                     1198.9(9)
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_collection       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-03 (Sheldrick, 2003)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7444
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.391
_diffrn_reflns_theta_min         2.196
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2882
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.6560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1127
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2117
_reflns_number_total             2882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b12607_si_006.cif
_cod_data_source_block           shelx
_cod_database_code               4125887
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.876
_shelx_estimated_absorpt_t_max   0.971
_shelx_res_checksum              55186
_shelx_hkl_checksum              14485