Brønsted acid-promoted C-F bond activation in [P,S]-ligated neutral and anionic perfluoronickelacyclopentanes.
Giffin, Kaitie A.; Korobkov, Ilia; Baker, R. Tom; Dalton transactions (Cambridge, England : 2003) 44 (2015) 19587–19596; doi:10.1039/c5dt02912k

data_7036663
_publ_section_title
;
 Br\/onsted acid-promoted C-F bond activation in [P,S]-ligated neutral and
 anionic perfluoronickelacyclopentanes.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19587
_journal_page_last               19596
_journal_paper_doi               10.1039/c5dt02912k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C47 H64 F8 N0 Na Ni O9 P S'
_chemical_formula_weight         1069.71
_chemical_name_systematic
'[1,2,4-(S),(Ph2P),Me(C6H3)]Ni(C4F8)(Na)(18-Crown-6)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-07-22 deposited with the CCDC.
2015-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.6427(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.8948(6)
_cell_length_b                   13.9815(4)
_cell_length_c                   34.7205(10)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.22
_cell_volume                     10800.6(5)
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_collection       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_molecular_graphics    'SHELXTL, Bruker (2004)'
_computing_publication_material  'SHELXTL, Bruker (2004)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-03 (Sheldrick, 2003)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.670
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_laue_measured_fraction_full 0.670
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            57572
_diffrn_reflns_point_group_measured_fraction_full 0.670
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         21.966
_diffrn_reflns_theta_min         1.720
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4480
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         6544
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0673
_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^)+(0.1110P)^2^+35.3010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.1893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5217
_reflns_number_total             6544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02912k2.cif
_cod_data_source_block           tb125
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7036657--7036663.cif.
;
_cod_database_code               7036663
_shelx_estimated_absorpt_t_min   0.896
_shelx_estimated_absorpt_t_max   0.960
_shelxl_version_number           2013-4
_shelx_res_checksum              94269