2,2,3,3-Tetrafluoronickelacyclopentanes Generated via the Oxidative Cyclization of Tetrafluoroethylene and Simple Alkenes: A Key Intermediate in Nickel-Catalyzed C‒C Bond-Forming Reactions
Ohashi, Masato; Kawashima, Takuya; Taniguchi, Tomoaki; Kikushima, Kotaro; Ogoshi, Sensuke; Organometallics 34 (2015) 1604–; doi:10.1021/acs.organomet.5b00218

data_4087522
_publ_section_title
;
 2,2,3,3-Tetrafluoronickelacyclopentanes Generated via the Oxidative
 Cyclization of Tetrafluoroethylene and Simple Alkenes: A Key Intermediate
 in Nickel-Catalyzed C--C Bond-Forming Reactions
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1604
_journal_paper_doi               10.1021/acs.organomet.5b00218
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C30 H43 F4 Ni O P'
_chemical_formula_sum            'C30 H43 F4 Ni O P'
_chemical_formula_weight         585.32
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.843(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.074(5)
_cell_length_b                   10.365(3)
_cell_length_c                   17.929(4)
_cell_measurement_reflns_used    6461
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.47
_cell_measurement_theta_min      3.05
_cell_volume                     2887.4(14)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalMaker for Windows ver. 2.7.6'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013) and modified'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Sir2011 (Murla, et al., 2012)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_unetI/netI     0.0875
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.970
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_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19125
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.455
_diffrn_reflns_theta_min         3.040
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1999). Abscor - Empirical Absorption Correction based on
Fourier Series Approximation. Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         6396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4239
_reflns_number_total             6396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00218_si_002.cif
_cod_data_source_block           Complx10
_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/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/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 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2887.5(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4087522
_shelx_estimated_absorpt_t_min   0.801
_shelx_estimated_absorpt_t_max   0.861
_shelxl_version_number           2013-4
_shelx_res_checksum              36822
_shelx_hkl_checksum              73620