Pentanuclear Nickel(II) Complex with two Vertex-Shared Triaminoguanidine Fragments and Symmetric Capping Ligand
Michael Böhme; Adrian E. Ion; Benjamin Kintzel; Axel Buchholz; Helmar Görls; Winfried Plass; Zeitschrift fuer Anorganische und Allgemeine Chemie 646 (2020) 999–1009; doi:10.1002/zaac.202000054

data_1573818
_publ_section_title
;
 Pentanuclear Nickel(II) Complex with two Vertex-Shared Triaminoguanidine
 Fragments and Symmetric Capping Ligand
;
_journal_issue                   13
_journal_name_full
'Zeitschrift fuer Anorganische und Allgemeine Chemie'
_journal_page_first              999
_journal_page_last               1009
_journal_paper_doi               10.1002/zaac.202000054
_journal_volume                  646
_journal_year                    2020
_chemical_formula_moiety         'C76 H48 Br3 N24 Ni3 O3, N O3 [+ solvent]'
_chemical_formula_sum            'C76 H48 Br3 N25 Ni3 O6'
_chemical_formula_weight         1823.25
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   22.1327(5)
_cell_length_b                   22.1327(5)
_cell_length_c                   65.0522(13)
_cell_measurement_reflns_used    60181
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.481
_cell_measurement_theta_min      2.215
_cell_volume                     27597.0(10)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi + omega - scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0832
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       84
_diffrn_reflns_limit_l_min       -84
_diffrn_reflns_number            60181
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         2.215
_exptl_absorpt_coefficient_mu    1.970
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             10992
_exptl_crystal_size_max          0.082
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.054
_refine_diff_density_max         1.728
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         7038
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1034P)^2^+65.6483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1794
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4447
_reflns_number_total             7038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Ni5.cif
_cod_data_source_block           FO2972
_cod_original_cell_volume        27597.0(14)
_cod_database_code               1573818
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.855
_shelx_estimated_absorpt_t_max   0.901
_shelx_res_checksum              8016
_shelx_hkl_checksum              57178
_shelx_fab_checksum              50440