Geometric and Electronic Structures of Nickel(II) Complexes of Redox Noninnocent Tetradentate Phenylenediamine Ligands.
Ciccione, Jérémie; Leconte, Nicolas; Luneau, Dominique; Philouze, Christian; Thomas, Fabrice; Inorganic chemistry 55 (2016) 649–665; doi:10.1021/acs.inorgchem.5b01947

data_4344588
_publ_section_title
;
 Geometric and Electronic Structures of Nickel(II) Complexes of Redox
 Noninnocent Tetradentate Phenylenediamine Ligands.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              649
_journal_page_last               665
_journal_paper_doi               10.1021/acs.inorgchem.5b01947
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'F6 Sb, C48 H58 N4 Ni O2'
_chemical_formula_sum            'C48 H58 F6 N4 Ni O2 Sb'
_chemical_formula_weight         1017.44
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-02-06
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.66(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.493(3)
_cell_length_b                   16.739(3)
_cell_length_c                   19.864(4)
_cell_measurement_temperature    200
_cell_volume                     4701.8(17)
_computing_cell_refinement       'Bruker Enraf Nonius kappa CCD'
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_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      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            KappaCCD
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker AXS enraf nonius KappaCCD'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_collimation    '0.2 mm sinlge-pinhole'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            50157
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.10
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_source_target            Mo
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.040
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.760732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.0607 before and 0.0319 after correction.
The Ratio of minimum to maximum transmission is 0.7607.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         13658
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+5.3426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                8779
_reflns_number_total             13658
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01947_si_001.cif
_cod_data_source_block           4b+
_cod_original_cell_volume        4701.9(16)
_cod_database_code               4344588