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_4341377
_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         'C36 H44 Br1 N4 Ni2,0.5(C6 H6)'
_chemical_formula_sum            'C39 H47 Br N4 Ni2'
_chemical_formula_weight         769.13
_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_method           SHELXL-2014/7
_cell_angle_alpha                109.523(3)
_cell_angle_beta                 110.713(3)
_cell_angle_gamma                90.321(2)
_cell_formula_units_Z            4
_cell_length_a                   15.5036(6)
_cell_length_b                   16.0481(5)
_cell_length_c                   17.7619(8)
_cell_measurement_reflns_used    78721
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      67.930
_cell_measurement_theta_min      4.556
_cell_volume                     3857.3(3)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.955
_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 HKL3000/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  0.085
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            78721
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.930
_diffrn_reflns_theta_min         4.556
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    2.649
_exptl_absorpt_correction_T_max  0.589
_exptl_absorpt_correction_T_min  0.007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.449
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     850
_refine_ls_number_reflns         13397
_refine_ls_number_restraints     600
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1909P)^2^+2.4909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2385
_refine_ls_wR_factor_ref         0.2506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11582
_reflns_number_total             13397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5020785_si_002.cif
_cod_data_source_block           CU007
_cod_depositor_comments
'Adding full bibliography for 4341373--4341379.cif.'
_cod_database_code               4341377
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              249
_shelx_hkl_checksum              97934
_shelx_fab_checksum              89637