#------------------------------------------------------------------------------
#$Date: 2025-08-19 16:18:28 +0300 (Tue, 19 Aug 2025) $
#$Revision: 301805 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/22/62/2226251.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2226251
loop_
_publ_author_name
'Wen, Changchun'
'Lu, Jianqi'
'Zhang, Zhong'
_publ_section_title
;
 Triaqua(1,4,7-triazacyclononane-κ³N¹,N⁴,N⁷)nickel(II)
 bromide nitrate
;
_journal_coeditor_code           PB2027
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m624
_journal_page_last               m625
_journal_paper_doi               10.1107/S160053681001620X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ni (C6 H15 N3) (H2 O)3] Br (N O3)'
_chemical_formula_moiety         'C6 H21 N3 Ni O3, N O3, Br'
_chemical_formula_sum            'C6 H21 Br N4 Ni O6'
_chemical_formula_weight         383.89
_chemical_name_systematic
;
Triaqua(1,4,7-triazacyclononane-
κ³N¹,N⁴,N⁷)nickel(II) bromide nitrate
;
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3000(10)
_cell_length_b                   11.3000(10)
_cell_length_c                   11.3000(10)
_cell_measurement_reflns_used    13409
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      3.12
_cell_volume                     1442.9(2)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'APEX2 (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15223
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    4.138
_exptl_absorpt_correction_T_max  0.480
_exptl_absorpt_correction_T_min  0.320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.465
_refine_ls_abs_structure_details 'Flack (1983), 475 Friedel pairs'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         8717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0232P)²+1.6516P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                985
_reflns_number_total             1110
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pb2027.cif
_cod_data_source_block           I
_cod_original_cell_volume        1442.9(3)
_cod_database_code               2226251
_cod_database_fobs_code          2226251
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 1.06169(4) 0.56169(4) 0.93831(4) 0.02729(19) Uani d S 1 . .
Br Br1 0.25347(4) 0.24653(4) 0.75347(4) 0.0437(2) Uani d S 1 . .
C C1 0.8566(4) 0.4233(4) 0.8872(4) 0.0437(11) Uani d . 1 . .
H H1A 0.8123 0.3498 0.8858 0.052 Uiso calc R 1 . .
H H1B 0.8438 0.4636 0.8125 0.052 Uiso calc R 1 . .
C C2 1.0118(4) 0.3128(4) 0.9995(4) 0.0449(11) Uani d . 1 . .
H H2A 1.0326 0.2365 0.9660 0.054 Uiso calc R 1 . .
H H2B 0.9417 0.3022 1.0478 0.054 Uiso calc R 1 . .
N N1 0.9850(3) 0.3973(3) 0.9019(3) 0.0353(8) Uani d . 1 . .
H H3 1.0226 0.3631 0.8407 0.053 Uiso d . 1 . .
N N2 0.9466(3) 0.9466(3) 0.9466(3) 0.0316(11) Uani d S 1 . .
O O1 1.0196(3) 0.6447(3) 0.7786(3) 0.0391(8) Uani d . 1 . .
O O2 0.8854(3) 1.0345(3) 0.9196(3) 0.0577(9) Uani d . 1 . .
H H4B 0.947(5) 0.659(4) 0.765(4) 0.050(14) Uiso d . 1 . .
H H4A 1.040(4) 0.598(4) 0.723(4) 0.050(14) Uiso d . 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ni1 0.02729(19) 0.02729(19) 0.02729(19) -0.0011(2) 0.0011(2) 0.0011(2)
Br1 0.0437(2) 0.0437(2) 0.0437(2) -0.0012(2) 0.0012(2) -0.0012(2)
C1 0.041(2) 0.042(3) 0.049(3) -0.016(2) -0.009(2) 0.005(2)
C2 0.054(3) 0.027(2) 0.054(3) -0.0022(19) 0.010(2) 0.0063(19)
N1 0.0365(19) 0.0349(19) 0.0346(19) -0.0022(14) 0.0050(14) -0.0021(14)
N2 0.0316(11) 0.0316(11) 0.0316(11) 0.0002(15) 0.0002(15) 0.0002(15)
O1 0.0424(18) 0.0419(18) 0.0330(18) 0.0052(14) -0.0007(13) 0.0024(12)
O2 0.055(2) 0.054(2) 0.065(2) 0.0156(16) 0.0149(17) 0.0133(18)
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Ni1 O1 11_567 . 84.90(14) ?
O1 Ni1 O1 11_567 8_746 84.90(14) ?
O1 Ni1 O1 . 8_746 84.90(14) ?
O1 Ni1 N1 11_567 . 177.00(13) ?
O1 Ni1 N1 . . 97.72(13) ?
O1 Ni1 N1 8_746 . 93.87(12) ?
O1 Ni1 N1 11_567 8_746 93.87(12) ?
O1 Ni1 N1 . 8_746 177.00(13) ?
O1 Ni1 N1 8_746 8_746 97.72(12) ?
N1 Ni1 N1 . 8_746 83.58(14) ?
O1 Ni1 N1 11_567 11_567 97.72(12) ?
O1 Ni1 N1 . 11_567 93.87(12) ?
O1 Ni1 N1 8_746 11_567 177.00(13) ?
N1 Ni1 N1 . 11_567 83.58(14) ?
N1 Ni1 N1 8_746 11_567 83.58(14) ?
N1 C1 C2 . 11_567 110.3(4) ?
N1 C1 H1A . . 109.6 ?
C2 C1 H1A 11_567 . 109.6 ?
N1 C1 H1B . . 109.6 ?
C2 C1 H1B 11_567 . 109.6 ?
H1A C1 H1B . . 108.1 ?
N1 C2 C1 . 8_746 111.7(3) ?
N1 C2 H2A . . 109.3 ?
C1 C2 H2A 8_746 . 109.3 ?
N1 C2 H2B . . 109.3 ?
C1 C2 H2B 8_746 . 109.3 ?
H2A C2 H2B . . 108.0 ?
C1 N1 C2 . . 114.0(3) ?
C1 N1 Ni1 . . 104.5(3) ?
C2 N1 Ni1 . . 109.8(3) ?
C1 N1 H3 . . 117.3 ?
C2 N1 H3 . . 101.4 ?
Ni1 N1 H3 . . 109.7 ?
O2 N2 O2 5 9 119.999(2) ?
O2 N2 O2 5 . 120.000(3) ?
O2 N2 O2 9 . 120.000(2) ?
Ni1 O1 H4B . . 117(4) ?
Ni1 O1 H4A . . 107(4) ?
H4B O1 H4A . . 104(5) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 O1 11_567 2.089(3) ?
Ni1 O1 . 2.089(3) ?
Ni1 O1 8_746 2.089(3) ?
Ni1 N1 . 2.091(3) ?
Ni1 N1 8_746 2.091(3) ?
Ni1 N1 11_567 2.091(3) ?
C1 N1 . 1.490(6) ?
C1 C2 11_567 1.520(6) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C2 N1 . 1.490(5) ?
C2 C1 8_746 1.520(6) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
N1 H3 . 0.8987 ?
N2 O2 5 1.248(3) ?
N2 O2 9 1.248(3) ?
N2 O2 . 1.248(3) ?
O1 H4B . 0.85(5) ?
O1 H4A . 0.84(4) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H4A O2 3_746 0.84(4) 1.95(5) 2.776(5) 162(4)
O1 H4B Br1 3_656 0.85(5) 2.48(5) 3.312(3) 167(4)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C2 C1 N1 C2 11_567 . . . 72.1(5) ?
C2 C1 N1 Ni1 11_567 . . . -47.8(4) ?
C1 C2 N1 C1 8_746 . . . -133.2(4) ?
C1 C2 N1 Ni1 8_746 . . . -16.3(4) ?
O1 Ni1 N1 C1 . . . . -62.7(3) ?
O1 Ni1 N1 C1 8_746 . . . -148.0(3) ?
N1 Ni1 N1 C1 8_746 . . . 114.6(2) ?
N1 Ni1 N1 C1 11_567 . . . 30.4(3) ?
O1 Ni1 N1 C2 . . . . 174.6(3) ?
O1 Ni1 N1 C2 8_746 . . . 89.3(3) ?
N1 Ni1 N1 C2 8_746 . . . -8.1(3) ?
N1 Ni1 N1 C2 11_567 . . . -92.3(2) ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168309845
