#------------------------------------------------------------------------------
#$Date: 2025-08-20 21:19:29 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301836 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/21/4302181.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_4302181
loop_
_publ_author_name
'Pampa Mukherjee'
'Michael G. B. Drew'
'Carlos J. Gómez-García'
'Ashutosh Ghosh'
_publ_section_title
;
(Ni2), (Ni3), and (Ni2+ Ni3): A Unique Example of Isolated and
Cocrystallized Ni2 and Ni3 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4817
_journal_page_last               4827
_journal_paper_doi               10.1021/ic802385c
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C26 H36 N4 Ni2 O6'
_chemical_formula_weight         618.00
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.77(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.056(5)
_cell_length_b                   16.355(3)
_cell_length_c                   8.5705(7)
_cell_measurement_reflns_used    6812
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.43
_cell_volume                     1369.0(7)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_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  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0903
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6812
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    1.422
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.712
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
_refine_ls_weighting_details 
  w=1/[σ²(Fo²)+(0.0826P)²+0.0000P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1447
_reflns_number_gt                2218
_reflns_number_total             3687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802385c_si_001_1.cif
_cod_data_source_block           1
_cod_original_cell_volume        1369.0(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4302181
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C13 C 1.2793(3) 0.8870(2) 0.2252(4) 0.0220(7) Uani 1 1 d . . .
H13 H 1.3248 0.9238 0.1734 0.026 Uiso 1 1 calc R . .
C14 C 1.3525(4) 0.8244(2) 0.3160(4) 0.0237(7) Uani 1 1 d . . .
H14 H 1.4461 0.8200 0.3241 0.028 Uiso 1 1 calc R . .
C15 C 1.2886(4) 0.7683(2) 0.3947(5) 0.0291(8) Uani 1 1 d . . .
H15 H 1.3384 0.7264 0.4552 0.035 Uiso 1 1 calc R . .
C16 C 1.1501(4) 0.7756(2) 0.3818(4) 0.0287(8) Uani 1 1 d . . .
H16 H 1.1075 0.7387 0.4365 0.034 Uiso 1 1 calc R . .
C17 C 1.0706(4) 0.8372(2) 0.2888(4) 0.0217(7) Uani 1 1 d . . .
C18 C 0.9270(4) 0.8405(2) 0.2979(4) 0.0261(8) Uani 1 1 d . . .
H18 H 0.8998 0.8054 0.3699 0.031 Uiso 1 1 calc R . .
C20 C 0.7000(4) 0.8916(2) 0.2516(5) 0.0293(8) Uani 1 1 d . . .
H20A H 0.6950 0.8493 0.3295 0.035 Uiso 1 1 calc R . .
H20B H 0.6292 0.8808 0.1551 0.035 Uiso 1 1 calc R . .
C21 C 0.6749(4) 0.9748(2) 0.3195(5) 0.0358(10) Uani 1 1 d . . .
H21A H 0.5864 0.9736 0.3460 0.043 Uiso 1 1 calc R . .
H21B H 0.7437 0.9834 0.4186 0.043 Uiso 1 1 calc R . .
C12 C 1.1373(4) 0.8959(2) 0.2097(4) 0.0211(7) Uani 1 1 d . . .
C22 C 0.6779(4) 1.0471(2) 0.2093(5) 0.0319(9) Uani 1 1 d . . .
H22A H 0.6078 1.0394 0.1109 0.038 Uiso 1 1 calc R . .
H22B H 0.6556 1.0963 0.2608 0.038 Uiso 1 1 calc R . .
C32 C 0.7216(4) 0.8789(2) -0.1777(4) 0.0261(8) Uani 1 1 d . . .
C34 C 0.6316(4) 0.8327(2) -0.3148(5) 0.0363(10) Uani 1 1 d . . .
H34A H 0.5596 0.8060 -0.2781 0.054 Uiso 1 1 calc R . .
H34B H 0.6852 0.7925 -0.3540 0.054 Uiso 1 1 calc R . .
H34C H 0.5925 0.8701 -0.3996 0.054 Uiso 1 1 calc R . .
C24 C 0.9216(4) 1.0812(2) 0.3115(5) 0.0330(9) Uani 1 1 d . . .
H23A H 0.8883 1.1232 0.3706 0.049 Uiso 1 1 calc R . .
H23B H 1.0005 1.1009 0.2783 0.049 Uiso 1 1 calc R . .
H23C H 0.9464 1.0340 0.3786 0.049 Uiso 1 1 calc R . .
O11 O 1.0702(2) 0.95738(13) 0.1229(3) 0.0214(5) Uani 1 1 d . . .
O31 O 0.8462(3) 0.85957(15) -0.1280(3) 0.0295(6) Uani 1 1 d . . .
O33 O 0.6699(3) 0.93570(15) -0.1125(3) 0.0269(6) Uani 1 1 d . . .
Ni1 Ni 0.86527(5) 0.96218(3) 0.03685(5) 0.02147(15) Uani 1 1 d . . .
N19 N 0.8350(3) 0.88864(18) 0.2133(4) 0.0249(7) Uani 1 1 d . . .
N23 N 0.8129(3) 1.05883(18) 0.1678(4) 0.0242(7) Uani 1 1 d . . .
H23 H 0.8025 1.1031 0.1015 0.029 Uiso 1 1 calc R . .
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'
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'
N N 0.0061 0.0033 '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
_geom_angle_publ_flag
C14 C13 C12 121.3(3) . . ?
C15 C14 C13 121.1(3) . . ?
C16 C15 C14 118.8(3) . . ?
C15 C16 C17 122.3(4) . . ?
C16 C17 C12 118.7(3) . . ?
C16 C17 C18 115.5(3) . . ?
C12 C17 C18 125.4(3) . . ?
N19 C18 C17 125.0(3) . . ?
N19 C20 C21 111.1(3) . . ?
C22 C21 C20 115.4(3) . . ?
O11 C12 C13 119.8(3) . . ?
O11 C12 C17 122.6(3) . . ?
C13 C12 C17 117.7(3) . . ?
N23 C22 C21 113.7(3) . . ?
O33 C32 O31 121.0(3) . . ?
O33 C32 C34 118.8(3) . . ?
O31 C32 C34 120.2(4) . . ?
C12 O11 Ni1 124.7(2) . . ?
C12 O11 Ni1 129.7(2) . 3_775 ?
Ni1 O11 Ni1 100.59(10) . 3_775 ?
C32 O31 Ni1 87.3(2) . . ?
C32 O33 Ni1 89.9(2) . . ?
N19 Ni1 O11 91.52(11) . . ?
N19 Ni1 N23 86.88(12) . . ?
O11 Ni1 N23 101.56(11) . . ?
N19 Ni1 O11 170.41(11) . 3_775 ?
O11 Ni1 O11 79.41(10) . 3_775 ?
N23 Ni1 O11 91.87(11) . 3_775 ?
N19 Ni1 O33 92.73(11) . . ?
O11 Ni1 O33 158.76(10) . . ?
N23 Ni1 O33 99.45(11) . . ?
O11 Ni1 O33 96.85(10) 3_775 . ?
N19 Ni1 O31 91.22(11) . . ?
O11 Ni1 O31 97.58(10) . . ?
N23 Ni1 O31 160.80(11) . . ?
O11 Ni1 O31 93.04(9) 3_775 . ?
O33 Ni1 O31 61.54(10) . . ?
C18 N19 C20 117.9(3) . . ?
C18 N19 Ni1 124.6(2) . . ?
C20 N19 Ni1 117.5(2) . . ?
C24 N23 C22 111.4(3) . . ?
C24 N23 Ni1 113.8(2) . . ?
C22 N23 Ni1 113.1(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C13 C14 1.387(5) . ?
C13 C12 1.410(5) . ?
C14 C15 1.384(5) . ?
C15 C16 1.376(6) . ?
C16 C17 1.408(5) . ?
C17 C12 1.432(5) . ?
C17 C18 1.465(5) . ?
C18 N19 1.297(5) . ?
C20 N19 1.471(4) . ?
C20 C21 1.525(5) . ?
C21 C22 1.518(5) . ?
C12 O11 1.334(4) . ?
C22 N23 1.496(5) . ?
C32 O33 1.259(4) . ?
C32 O31 1.263(4) . ?
C32 C34 1.504(5) . ?
C24 N23 1.485(5) . ?
O11 Ni1 2.018(3) . ?
O11 Ni1 2.109(2) 3_775 ?
O31 Ni1 2.172(3) . ?
O33 Ni1 2.118(3) . ?
Ni1 N19 2.012(3) . ?
Ni1 N23 2.078(3) . ?
Ni1 O11 2.109(2) 3_775 ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168336757
