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_4341379
_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         'C40 H50 Br2 N6 Ni2,F6 P1,0.795(C4 H10 O1)'
_chemical_formula_sum            'C43.18 H57.95 Br2 F6 N6 Ni2 O0.79 P'
_chemical_formula_weight         1095.91
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 100.166(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6267(3)
_cell_length_b                   31.1603(9)
_cell_length_c                   15.8194(5)
_cell_measurement_reflns_used    30853
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      66.594
_cell_measurement_theta_min      4.870
_cell_volume                     5156.1(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 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.923
_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  0.032
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30853
_diffrn_reflns_point_group_measured_fraction_full 0.903
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_min         4.870
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    3.505
_exptl_absorpt_correction_T_max  0.704
_exptl_absorpt_correction_T_min  0.001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2241
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         8415
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+10.9187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1590
_refine_ls_wR_factor_ref         0.1751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7324
_reflns_number_total             8415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5020785_si_002.cif
_cod_data_source_block           CU017
_cod_depositor_comments
'Adding full bibliography for 4341373--4341379.cif.'
_cod_database_code               4341379
_shelx_estimated_absorpt_t_min   0.474
_shelx_estimated_absorpt_t_max   0.721
_shelxl_version_number           2014-3
_shelx_res_checksum              52782
_shelx_hkl_checksum              21956
_shelx_fab_checksum              82434