Characterization of Intermediates in the C−F Activation of Tetrafluorobenzenes using a Reactive Ni(PEt3)2Synthon: Combined Computational and Experimental Investigation
Johnson, Samuel A.; Mroz, Natalia M.; Valdizon, René; Murray, Scott; Organometallics 30 (2011) 441–; doi:10.1021/om100699d

data_4063635
_publ_contact_author             'Samuel A. Johnson'
_publ_section_title
;
 Characterization of Intermediates in the C&#x2212;F Activation of
 Tetrafluorobenzenes using a Reactive Ni(PEt3)2Synthon: Combined
 Computational and Experimental Investigation
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              441
_journal_paper_doi               10.1021/om100699d
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C30 H61 F3 Ni2 P4'
_chemical_formula_sum            'C30 H61 F3 Ni2 P4'
_chemical_formula_weight         720.10
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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             2010-10-13T14:35:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                116.821(2)
_cell_angle_beta                 90.686(2)
_cell_angle_gamma                101.406(2)
_cell_formula_units_Z            4
_cell_length_a                   10.5150(14)
_cell_length_b                   19.138(3)
_cell_length_c                   20.958(3)
_cell_measurement_reflns_used    2
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      2.55
_cell_volume                     3664.7(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52454
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    1.235
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS, BRUKER 2001'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         52497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.865
_refine_ls_R_factor_all          0.067
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.094
_reflns_number_gt                34628
_reflns_number_total             52454
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100699d_si_002.cif
_cod_data_source_block           sj1245zm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4063635