Selective Catalytic Formation of Cross-Tetramers from Tetrafluoroethylene, Ethylene, Alkynes, and Aldehydes via Nickelacycles as Key Reaction Intermediates.
Kawashima, Takuya; Ohashi, Masato; Ogoshi, Sensuke; Journal of the American Chemical Society 140 (2018) 17423–17427; doi:10.1021/jacs.8b11671

data_4133614
_publ_section_title
;
 Selective Catalytic Formation of Cross-Tetramers from
 Tetrafluoroethylene, Ethylene, Alkynes, and Aldehydes via Nickelacycles
 as Key Reaction Intermediates.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17423
_journal_page_last               17427
_journal_paper_doi               10.1021/jacs.8b11671
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C35 H51 F4 Ni P, 0.5(C5 H12)'
_chemical_formula_sum            'C37.5 H57 F4 Ni P'
_chemical_formula_weight         673.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 94.7276(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7227(2)
_cell_length_b                   16.83446(17)
_cell_length_c                   11.12873(14)
_cell_measurement_reflns_used    19789
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      74.0750
_cell_measurement_theta_min      4.7430
_cell_volume                     3495.69(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Crystal Maker (ver. 2.7.6, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013) and modified'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            44838
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.285
_diffrn_reflns_theta_min         3.536
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.607
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.31d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
The unit cell contains 2 pentane molecules which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON.

TITL shelxl    P 21/c       R = 0.07
CELL   18.7227   16.8345   11.1287     90.00     94.73     90.00
SPGR P21/c
C101 0.918 0.594 0.062 !       3.30 eA-3
C102 0.026 0.983 0.482 !       3.04 eA-3
C103 0.915 0.958 0.501 !       2.75 eA-3
C104 0.031 0.065 0.504 !       1.24 eA-3

;
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         7074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0490P)^2^+0.8024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0880
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6444
_reflns_number_total             7074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b11671_si_002.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C37.50 H57 F4 Ni P'
_cod_database_code               4133614
_shelxl_version_number           2013-4
_shelx_res_checksum              23523
_shelx_hkl_checksum              22416
_shelx_fab_checksum              97223