New Dinuclear Nickel(II) Complexes: Synthesis, Structure, Electrochemical, and Magnetic Properties
Dmitry Yakhvarov; Ekaterina Trofimova; Oleg Sinyashin; Olga Kataeva; Yulia Budnikova; Peter Lönnecke; Evamarie Hey-Hawkins; Andreas Petr; Yulia Krupskaya; Vladislav Kataev; Rüdiger Klingeler; Bernd Büchner; Inorganic Chemistry 50 (2011) 4553–4558; doi:10.1021/ic2002546

data_4325076
_publ_section_title
;
 New Dinuclear Nickel(II) Complexes: Synthesis, Structure,
 Electrochemical, and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4553
_journal_page_last               4558
_journal_paper_doi               10.1021/ic2002546
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C74 H65.84 Br2.17 N10 Ni2 O6 P2'
_chemical_formula_weight         1543.57
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2009-09-25T16:51:58-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 103.476(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5067(5)
_cell_length_b                   21.2589(6)
_cell_length_c                   12.1901(4)
_cell_measurement_reflns_used    12144
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.3468
_cell_measurement_theta_min      2.866
_cell_volume                     3403.9(2)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_molecular_graphics
;
 ORTEP3 for Windows
 L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.
;
_computing_publication_material
;
 WINGX
 L.J. Farrugia,
 J. Appl. Cryst., 1999, 32, 837-838.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 SHELXS-97
 Program for Crystal Structure Analysis (Release 97-2)
 G. M. Sheldrick, Instit\"ut f\"ur Anorganische Chemie der Universit\"at,
 Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998.
;
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0488714708
_diffrn_orient_matrix_UB_12      -0.0075709109
_diffrn_orient_matrix_UB_13      0.0381509549
_diffrn_orient_matrix_UB_21      -0.0256086827
_diffrn_orient_matrix_UB_22      0.0126428953
_diffrn_orient_matrix_UB_23      0.0379150771
_diffrn_orient_matrix_UB_31      -0.0232077385
_diffrn_orient_matrix_UB_32      -0.0299158691
_diffrn_orient_matrix_UB_33      0.0061435841
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.069
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            39248
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.1
_exptl_absorpt_coefficient_mu    1.933
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.88668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
        empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       prism
_exptl_crystal_F_000             1579
_exptl_crystal_size_max          0.3455
_exptl_crystal_size_mid          0.1407
_exptl_crystal_size_min          0.0651
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.851
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         10353
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      0.85
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0646
_reflns_number_gt                6461
_reflns_number_total             10353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2002546_si_002.cif
_cod_data_source_block           x0835fin
_cod_original_cell_volume        3403.87(19)
_cod_database_code               4325076