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_4341378
_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_absolute_configuration ad
_chemical_formula_moiety         'C72 H88 Br5 N8 Ni4,F6 P1,2(C4 H10 O1)'
_chemical_formula_sum            'C80 H108 Br5 F6 N8 Ni4 O2 P'
_chemical_formula_weight         1993.10
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           79
_space_group_name_Hall           'I 4'
_space_group_name_H-M_alt        'I 4'
_symmetry_space_group_name_Hall  'I 4'
_symmetry_space_group_name_H-M   'I 4'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8162(2)
_cell_length_b                   16.8162(2)
_cell_length_c                   31.4122(7)
_cell_measurement_reflns_used    20749
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.091
_cell_measurement_theta_min      4.664
_cell_volume                     8882.9(2)
_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-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.968
_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  0.045
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            20749
_diffrn_reflns_point_group_measured_fraction_full 0.912
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.091
_diffrn_reflns_theta_min         4.664
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    4.240
_exptl_absorpt_correction_T_max  0.654
_exptl_absorpt_correction_T_min  0.159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       block
_exptl_crystal_F_000             4064
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Flack x determined using 3131 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.026(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7784
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0893P)^2^+30.9418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1604
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    0.833
_reflns_Friedel_fraction_max     0.802
_reflns_number_gt                7382
_reflns_number_total             7784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5020785_si_002.cif
_cod_data_source_block           CU016
_cod_depositor_comments
'Adding full bibliography for 4341373--4341379.cif.'
_cod_original_cell_volume        8882.9(3)
_cod_database_code               4341378
_shelx_estimated_absorpt_t_min   0.484
_shelx_estimated_absorpt_t_max   0.676
_shelxl_version_number           2014-3
_shelx_res_checksum              58953
_shelx_hkl_checksum              25381
_shelx_fab_checksum              90185