A T-shaped Ni[κ2-(CF2)4‒] NHC complex: unusual Csp3‒F and M‒CFbond functionalization reactions
Andrella, Nicholas O.; Sicard, Alexandre J.; Gorelsky, Serge I.; Korobkov, Ilia; Baker, R. Tom; Chem. Sci. 6 (2015) 6392–; doi:10.1039/C5SC01886B

data_1529367
_publ_section_title
;
 A T-shaped Ni[\k2-(CF2)4--] NHC complex: unusual Csp3--F and M--CFbond
 functionalization reactions
;
_journal_issue                   11
_journal_name_full               'Chem. Sci.'
_journal_page_first              6392
_journal_paper_doi               10.1039/C5SC01886B
_journal_volume                  6
_journal_year                    2015
_chemical_formula_sum            'C33 H41 F7 N2 Ni O2'
_chemical_formula_weight         689.39
_chemical_name_common            '[Ni[k3-(CF2)3CF(O2CCH3)-}(SIPr)] '
_chemical_name_systematic
; 
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-02-17 deposited with the CCDC.
2015-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.180(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7181(4)
_cell_length_b                   18.2160(7)
_cell_length_c                   19.2228(7)
_cell_measurement_reflns_used    5916
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      2.57
_cell_volume                     3400.5(2)
_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 0.791
_diffrn_measured_fraction_theta_max 0.977
_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_unetI/netI     0.0735
_diffrn_reflns_laue_measured_fraction_full 0.791
_diffrn_reflns_laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11781
_diffrn_reflns_point_group_measured_fraction_full 0.791
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.430
_diffrn_reflns_theta_min         1.541
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_max  0.744894
_exptl_absorpt_correction_T_min  0.535198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.423
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_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+11.4852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1475
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4696
_reflns_number_total             6216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc01886b2.cif
_cod_data_source_block           tb132_5
_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 1529364--1529368.cif.
;
_cod_database_code               1529367
_shelx_estimated_absorpt_t_min   0.916
_shelx_estimated_absorpt_t_max   0.945
_shelxl_version_number           2013-4
_shelx_res_checksum              67888