Nickel complexes of a binucleating ligand derived from an SCS pincer.
Peterson, Sonja M.; Helm, Monte L.; Appel, Aaron M.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 747–752; doi:10.1039/c4dt02718c

data_7033107
_publ_section_title
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 Nickel complexes of a binucleating ligand derived from an SCS pincer.
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_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              747
_journal_page_last               752
_journal_paper_doi               10.1039/c4dt02718c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C18 H23 Br F6 Li N Ni O7 S4'
_chemical_formula_sum            'C18 H23 Br F6 Li N Ni O7 S4'
_chemical_formula_weight         753.17
_chemical_name_systematic
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 [Ni(L)(mu-Br)Li]N(OTf)2 
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_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-01-21
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.11.06 svn.r2526, GUI svn.r4372)
;
_cell_angle_alpha                88.473(3)
_cell_angle_beta                 85.212(3)
_cell_angle_gamma                71.110(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0944(6)
_cell_length_b                   9.0875(6)
_cell_length_c                   19.2405(13)
_cell_measurement_reflns_used    513
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      2.60
_cell_volume                     1334.39(16)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      140.15
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22490
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         1.06
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.620
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0782 before and 0.0432 after correction.
The Ratio of minimum to maximum transmission is 0.7716.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+2.0725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0899
_reflns_number_gt                4902
_reflns_number_total             6216
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02718c2.cif
_cod_data_source_block           helm138_0m
_cod_depositor_comments
'Adding full bibliography for 7033106--7033107.cif.'
_cod_database_code               7033107
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  {H3A,H3B} of C3, H4 of C4, H5 of C5, H6 of C6, {H8A,H8B} of C8, {H9A,H9B}
  of C9, {H10A,H10B} of C10, {H11A,H11B} of C11, {H12A,H12B} of C12, {H13A,
  H13B} of C13, {H14A,H14B} of C14, {H15A,H15B} of C15, {H16A,H16B,H16C,H16D}
  of C16, {H15C,H15D} of C15A, {H14C,H14D} of C14A, {H13C,H13D} of C13A, {H11C,
  H11D} of C11A, {H12C,H12D} of C12A
2. Uiso/Uaniso restraints and constraints
Uanis(F2) = Uanis(F3A) = Uanis(F1A) = Uanis(F3) = Uanis(C17) = Uanis(C17A) = Uanis(F2A) = Uanis(F1)
3. Others
 Sof(O2)=Sof(O3)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H16A)=Sof(H16B)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-
 Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=
 1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-
 Sof(O3)=Sof(Li1A)
 Sof(F1)=Sof(F2)=1-Sof(F2)=1-Sof(F2)=1-Sof(F2)=Sof(F1A)=1-Sof(F2)=Sof(C17A)
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C16(H16C,H16D), C15A(H15C,H15D), C14A(H14C,H14D), C13A(H13C,H13D), C11A(H11C,
 H11D), C12A(H12C,H12D)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6)
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