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#$Date: 2025-01-31 21:16:40 +0200 (Fri, 31 Jan 2025) $
#$Revision: 297545 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573818.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1573818
loop_
_publ_author_name
'Michael Böhme'
'Adrian E. Ion'
'Benjamin Kintzel'
'Axel Buchholz'
'Helmar Görls'
'Winfried Plass'
_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/[σ²(Fo²)+(0.1034P)²+65.6483P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.855
_shelx_estimated_absorpt_t_max   0.901
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni -0.19568(2) 0.44982(2) -0.04655(2) 0.03849(16) Uani 1 1 d . . . . .
Br Br -0.23575(3) 0.76434(3) -0.05797(2) 0.0836(2) Uani 1 1 d . . . . .
O1 O -0.14613(14) 0.55283(14) -0.04055(5) 0.0481(7) Uani 1 1 d . . . . .
N1 N -0.34613(15) 0.38688(15) -0.05218(5) 0.0373(7) Uani 1 1 d . . . . .
N2 N -0.28483(15) 0.45108(15) -0.05062(5) 0.0367(7) Uani 1 1 d . . . . .
N3 N -0.19125(17) 0.42904(17) -0.01390(5) 0.0437(8) Uani 1 1 d . . . . .
N4 N -0.10518(16) 0.45018(16) -0.04339(5) 0.0404(7) Uani 1 1 d . . . . .
N5 N -0.02868(18) 0.43098(19) -0.02281(6) 0.0493(8) Uani 1 1 d . . . . .
N6 N -0.00170(17) 0.46517(18) -0.05808(6) 0.0476(8) Uani 1 1 d . . . . .
N7 N -0.15216(17) 0.46964(17) -0.07749(5) 0.0428(7) Uani 1 1 d . . . . .
N8 N 0.0862(2) 0.4183(2) -0.01997(6) 0.0578(10) Uani 1 1 d . . . . .
C1 C -0.333333 0.333333 -0.05200(10) 0.0354(13) Uani 1 3 d S T P . .
C2 C -0.2897(2) 0.5052(2) -0.05476(6) 0.0430(9) Uani 1 1 d . . . . .
H2A H -0.333060 0.497493 -0.060014 0.052 Uiso 1 1 calc R U . . .
C3 C -0.2348(2) 0.5772(2) -0.05212(6) 0.0449(9) Uani 1 1 d . . . . .
C4 C -0.2543(2) 0.6281(2) -0.05618(8) 0.0561(11) Uani 1 1 d . . . . .
H4A H -0.299448 0.614239 -0.061453 0.067 Uiso 1 1 calc R U . . .
C5 C -0.2085(3) 0.6968(2) -0.05251(9) 0.0649(13) Uani 1 1 d . . . . .
C6 C -0.1433(3) 0.7177(2) -0.04443(9) 0.0727(15) Uani 1 1 d . . . . .
H6A H -0.112254 0.765666 -0.041595 0.087 Uiso 1 1 calc R U . . .
C7 C -0.1236(2) 0.6696(2) -0.04051(9) 0.0642(13) Uani 1 1 d . . . . .
H7A H -0.078572 0.684713 -0.034935 0.077 Uiso 1 1 calc R U . . .
C8 C -0.1687(2) 0.5970(2) -0.04454(7) 0.0485(10) Uani 1 1 d . . . . .
C9 C -0.2362(2) 0.4214(2) 0.00067(7) 0.0513(10) Uani 1 1 d . . . . .
H9A H -0.274415 0.427683 -0.002767 0.062 Uiso 1 1 calc R U . . .
C10 C -0.2296(2) 0.4045(2) 0.02097(7) 0.0544(11) Uani 1 1 d . . . . .
H10A H -0.262440 0.399936 0.031123 0.065 Uiso 1 1 calc R U . . .
C11 C -0.1750(2) 0.3944(2) 0.02599(7) 0.0547(11) Uani 1 1 d . . . . .
H11A H -0.170478 0.381681 0.039606 0.066 Uiso 1 1 calc R U . . .
C12 C -0.1266(2) 0.4031(2) 0.01109(6) 0.0512(10) Uani 1 1 d . . . . .
H12A H -0.088211 0.396676 0.014228 0.061 Uiso 1 1 calc R U . . .
C13 C -0.1359(2) 0.4213(2) -0.00849(6) 0.0460(9) Uani 1 1 d . . . . .
C14 C -0.0862(2) 0.4355(2) -0.02557(6) 0.0460(9) Uani 1 1 d . . . . .
C15 C -0.0612(2) 0.4655(2) -0.05902(6) 0.0440(9) Uani 1 1 d . . . . .
C16 C 0.0112(2) 0.4459(2) -0.03957(7) 0.0475(10) Uani 1 1 d . . . . .
C17 C 0.0753(2) 0.4404(2) -0.03821(7) 0.0517(10) Uani 1 1 d . . . . .
C18 C 0.1200(2) 0.4566(3) -0.05456(8) 0.0610(12) Uani 1 1 d . . . . .
H18A H 0.110600 0.471443 -0.067261 0.073 Uiso 1 1 calc R U . . .
C19 C 0.1795(3) 0.4509(3) -0.05218(9) 0.0681(14) Uani 1 1 d . . . . .
H19A H 0.211872 0.463121 -0.063143 0.082 Uiso 1 1 calc R U . . .
C20 C 0.1908(3) 0.4277(3) -0.03397(9) 0.0690(14) Uani 1 1 d . . . . .
H20A H 0.230350 0.422064 -0.032150 0.083 Uiso 1 1 calc R U . . .
C21 C 0.1433(3) 0.4124(3) -0.01817(9) 0.0682(14) Uani 1 1 d . . . . .
H21A H 0.151584 0.396936 -0.005420 0.082 Uiso 1 1 calc R U . . .
C22 C -0.0872(2) 0.4781(2) -0.07851(6) 0.0449(9) Uani 1 1 d . . . . .
C23 C -0.0495(2) 0.4941(2) -0.09684(7) 0.0515(10) Uani 1 1 d . . . . .
H23A H -0.003376 0.501399 -0.096960 0.062 Uiso 1 1 calc R U . . .
C24 C -0.0793(3) 0.4991(3) -0.11443(7) 0.0638(13) Uani 1 1 d . . . . .
H24A H -0.054074 0.510689 -0.127000 0.077 Uiso 1 1 calc R U . . .
C25 C -0.1475(3) 0.4871(3) -0.11391(8) 0.0675(14) Uani 1 1 d . . . . .
H25A H -0.170312 0.488211 -0.126150 0.081 Uiso 1 1 calc R U . . .
C26 C -0.1815(3) 0.4733(3) -0.09475(7) 0.0585(12) Uani 1 1 d . . . . .
H26A H -0.227441 0.466381 -0.094236 0.070 Uiso 1 1 calc R U . . .
N1N N -0.333333 0.6267(3) 0.083333 0.0387(14) Uani 0.6667 2 d S TU P . .
O1N O -0.333333 0.6918(5) 0.083333 0.117(3) Uani 0.6667 2 d S TU P . .
O2N O -0.3436(4) 0.5892(5) 0.06433(13) 0.124(3) Uani 0.6667 1 d . U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N2 Ni N4 178.05(13) . .
N2 Ni O1 89.57(12) . .
N4 Ni O1 89.90(12) . .
N2 Ni N1 77.38(12) . 3_455
N4 Ni N1 103.22(12) . 3_455
O1 Ni N1 166.72(12) . 3_455
N2 Ni N7 102.37(12) . .
N4 Ni N7 75.76(12) . .
O1 Ni N7 90.88(12) . .
N1 Ni N7 94.30(13) 3_455 .
N2 Ni N3 106.23(12) . .
N4 Ni N3 75.64(12) . .
O1 Ni N3 89.64(12) . .
N1 Ni N3 91.62(12) 3_455 .
N7 Ni N3 151.40(12) . .
C8 O1 Ni 127.1(3) . .
C1 N1 N2 111.7(2) . .
C1 N1 Ni 112.22(18) . 2_565
N2 N1 Ni 133.4(2) . 2_565
C2 N2 N1 116.3(3) . .
C2 N2 Ni 125.7(3) . .
N1 N2 Ni 117.3(2) . .
C9 N3 C13 117.7(4) . .
C9 N3 Ni 127.8(3) . .
C13 N3 Ni 114.5(3) . .
C14 N4 C15 116.7(3) . .
C14 N4 Ni 121.7(3) . .
C15 N4 Ni 121.6(3) . .
C16 N5 C14 114.0(4) . .
C15 N6 C16 114.2(4) . .
C26 N7 C22 118.0(4) . .
C26 N7 Ni 128.1(3) . .
C22 N7 Ni 113.9(3) . .
C21 N8 C17 117.4(4) . .
N1 C1 N1 119.999(14) 3_455 2_565
N1 C1 N1 119.989(15) 3_455 .
N1 C1 N1 119.989(15) 2_565 .
N2 C2 C3 125.7(4) . .
N2 C2 H2A 117.1 . .
C3 C2 H2A 117.1 . .
C8 C3 C4 120.4(4) . .
C8 C3 C2 124.0(4) . .
C4 C3 C2 115.4(4) . .
C5 C4 C3 120.0(4) . .
C5 C4 H4A 120.0 . .
C3 C4 H4A 120.0 . .
C4 C5 C6 120.8(4) . .
C4 C5 Br 119.4(4) . .
C6 C5 Br 119.7(3) . .
C7 C6 C5 119.9(4) . .
C7 C6 H6A 120.1 . .
C5 C6 H6A 120.1 . .
C6 C7 C8 121.9(4) . .
C6 C7 H7A 119.1 . .
C8 C7 H7A 119.1 . .
O1 C8 C3 124.2(4) . .
O1 C8 C7 118.9(4) . .
C3 C8 C7 116.9(4) . .
N3 C9 C10 122.5(4) . .
N3 C9 H9A 118.8 . .
C10 C9 H9A 118.8 . .
C11 C10 C9 119.1(4) . .
C11 C10 H10A 120.4 . .
C9 C10 H10A 120.4 . .
C10 C11 C12 119.6(4) . .
C10 C11 H11A 120.2 . .
C12 C11 H11A 120.2 . .
C13 C12 C11 117.8(4) . .
C13 C12 H12A 121.1 . .
C11 C12 H12A 121.1 . .
N3 C13 C12 123.3(4) . .
N3 C13 C14 113.4(3) . .
C12 C13 C14 123.3(4) . .
N4 C14 N5 124.4(4) . .
N4 C14 C13 114.4(3) . .
N5 C14 C13 121.1(4) . .
N6 C15 N4 124.6(4) . .
N6 C15 C22 121.7(4) . .
N4 C15 C22 113.5(3) . .
N5 C16 N6 125.9(4) . .
N5 C16 C17 118.1(4) . .
N6 C16 C17 116.0(4) . .
N8 C17 C18 122.7(4) . .
N8 C17 C16 115.6(4) . .
C18 C17 C16 121.7(4) . .
C17 C18 C19 118.7(5) . .
C17 C18 H18A 120.6 . .
C19 C18 H18A 120.6 . .
C20 C19 C18 119.5(5) . .
C20 C19 H19A 120.3 . .
C18 C19 H19A 120.3 . .
C19 C20 C21 118.3(5) . .
C19 C20 H20A 120.8 . .
C21 C20 H20A 120.8 . .
N8 C21 C20 123.4(5) . .
N8 C21 H21A 118.3 . .
C20 C21 H21A 118.3 . .
N7 C22 C23 122.4(4) . .
N7 C22 C15 114.8(3) . .
C23 C22 C15 122.7(4) . .
C24 C23 C22 119.2(4) . .
C24 C23 H23A 120.4 . .
C22 C23 H23A 120.4 . .
C23 C24 C25 119.3(5) . .
C23 C24 H24A 120.4 . .
C25 C24 H24A 120.4 . .
C24 C25 C26 118.2(5) . .
C24 C25 H25A 120.9 . .
C26 C25 H25A 120.9 . .
N7 C26 C25 122.7(5) . .
N7 C26 H26A 118.7 . .
C25 C26 H26A 118.7 . .
O1N N1N O2N 119.8(5) . .
O1N N1N O2N 119.8(5) . 18_444
O2N N1N O2N 120.4(9) . 18_444
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni N2 2.005(3) .
Ni N4 2.010(3) .
Ni O1 2.013(3) .
Ni N1 2.066(3) 3_455
Ni N7 2.179(3) .
Ni N3 2.186(3) .
Br C5 1.905(5) .
O1 C8 1.326(5) .
N1 C1 1.349(3) .
N1 N2 1.394(4) .
N2 C2 1.284(5) .
N3 C9 1.322(5) .
N3 C13 1.365(5) .
N4 C14 1.328(5) .
N4 C15 1.329(5) .
N5 C16 1.336(6) .
N5 C14 1.337(5) .
N6 C15 1.321(5) .
N6 C16 1.355(6) .
N7 C26 1.320(6) .
N7 C22 1.355(5) .
N8 C21 1.339(6) .
N8 C17 1.349(6) .
C2 C3 1.452(5) .
C2 H2A 0.9500 .
C3 C8 1.391(6) .
C3 C4 1.419(6) .
C4 C5 1.363(6) .
C4 H4A 0.9500 .
C5 C6 1.379(7) .
C6 C7 1.363(7) .
C6 H6A 0.9500 .
C7 C8 1.430(6) .
C7 H7A 0.9500 .
C9 C10 1.400(6) .
C9 H9A 0.9500 .
C10 C11 1.371(6) .
C10 H10A 0.9500 .
C11 C12 1.386(6) .
C11 H11A 0.9500 .
C12 C13 1.382(6) .
C12 H12A 0.9500 .
C13 C14 1.483(6) .
C15 C22 1.476(6) .
C16 C17 1.488(6) .
C17 C18 1.373(7) .
C18 C19 1.391(7) .
C18 H18A 0.9500 .
C19 C20 1.364(8) .
C19 H19A 0.9500 .
C20 C21 1.387(7) .
C20 H20A 0.9500 .
C21 H21A 0.9500 .
C22 C23 1.397(6) .
C23 C24 1.353(7) .
C23 H23A 0.9500 .
C24 C25 1.396(8) .
C24 H24A 0.9500 .
C25 C26 1.408(7) .
C25 H25A 0.9500 .
C26 H26A 0.9500 .
N1N O1N 1.439(13) .
N1N O2N 1.442(9) .
N1N O2N 1.442(9) 18_444
