Dinuclear nickel complexes in five States of oxidation using a redox-active ligand.
Zhou, You-Yun; Hartline, Douglas R.; Steiman, Talia J.; Fanwick, Phillip E.; Uyeda, Christopher; Inorganic chemistry 53 (2014) 11770–11777; doi:10.1021/ic5020785

data_4341374
_publ_section_title
;
 Dinuclear nickel complexes in five States of oxidation using a
 redox-active ligand.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11770
_journal_page_last               11777
_journal_paper_doi               10.1021/ic5020785
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C42 H50 N4 Ni2'
_chemical_formula_sum            'C42 H50 N4 Ni2'
_chemical_formula_weight         728.28
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   37.6344(14)
_cell_length_b                   37.6344(14)
_cell_length_c                   14.6022(10)
_cell_measurement_reflns_used    34402
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      69.979
_cell_measurement_theta_min      2.348
_cell_volume                     17911.0(15)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR2004 (Burla, et. al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not 
cusp data but mostly high angle data.
Also the use of HKL2000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total.
;
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34402
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.979
_diffrn_reflns_theta_min         2.348
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    1.409
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       needle
_exptl_crystal_F_000             6948
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         7320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+173.9251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5217
_reflns_number_total             7320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5020785_si_002.cif
_cod_data_source_block           CU001
_cod_depositor_comments
'Adding full bibliography for 4341373--4341379.cif.'
_cod_original_cell_volume        17911.0(18)
_cod_database_code               4341374
_shelxl_version_number           2013-4
_shelx_res_checksum              7001
_shelx_hkl_checksum              8402
_shelx_fab_checksum              47735