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_1573819
_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         'C116 H72 Br6 N36 Ni5 O6 [+ solvent]'
_chemical_formula_sum            'C116 H72 Br6 N36 Ni5 O6'
_chemical_formula_weight         2838.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                101.424(1)
_cell_angle_beta                 98.074(1)
_cell_angle_gamma                110.463(1)
_cell_formula_units_Z            2
_cell_length_a                   16.5193(4)
_cell_length_b                   16.7116(3)
_cell_length_c                   27.7661(7)
_cell_measurement_reflns_used    44017
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.489
_cell_measurement_theta_min      1.722
_cell_volume                     6853.3(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.1255
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            44017
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         1.722
_exptl_absorpt_coefficient_mu    2.484
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2836
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.818
_refine_diff_density_min         -1.595
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1522
_refine_ls_number_reflns         30908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1525
_refine_ls_R_factor_gt           0.0744
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+2.2443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.2000
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                15794
_reflns_number_total             30908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Ni5.cif
_cod_data_source_block           FO2628_Ni5
_cod_database_code               1573819
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.886
_shelx_estimated_absorpt_t_max   0.886
_shelx_res_checksum              63524
_shelx_hkl_checksum              91982
_shelx_fab_checksum              98419