#------------------------------------------------------------------------------
#$Date: 2025-08-20 21:19:29 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301836 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/21/4302182.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_4302182
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            'C33 H56 Cl2 N4 Ni3 O14'
_chemical_formula_weight         979.84
_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                 105.031(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4256(3)
_cell_length_b                   20.4513(7)
_cell_length_c                   10.8823(3)
_cell_measurement_reflns_used    14651
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.61
_cell_volume                     2240.90(12)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14651
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.61
_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    1.429
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.463
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         6445
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.000
_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)+(0.0567P)²+3.7473P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1443
_reflns_number_gt                4901
_reflns_number_total             6445
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802385c_si_001_2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4302182
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
C21 C 0.3674(3) 0.52809(19) 0.1124(3) 0.0273(7) Uani 1 1 d . . .
H21A H 0.4107 0.4914 0.1631 0.033 Uiso 1 1 calc R . .
H21B H 0.4132 0.5362 0.0469 0.033 Uiso 1 1 calc R . .
C32 C 0.3028(3) 0.52167(17) 0.6069(3) 0.0209(6) Uani 1 1 d . . .
C34 C 0.2888(3) 0.5123(2) 0.7404(3) 0.0279(7) Uani 1 1 d . . .
H34A H 0.3278 0.4713 0.7734 0.042 Uiso 1 1 calc R . .
H34B H 0.1964 0.5123 0.7391 0.042 Uiso 1 1 calc R . .
H34C H 0.3332 0.5472 0.7936 0.042 Uiso 1 1 calc R . .
C12 C -0.0067(3) 0.40007(16) 0.2822(3) 0.0204(6) Uani 1 1 d . . .
C13 C -0.0849(3) 0.35578(17) 0.3311(3) 0.0270(7) Uani 1 1 d . . .
H13 H -0.1009 0.3642 0.4098 0.032 Uiso 1 1 calc R . .
C14 C -0.1384(4) 0.3003(2) 0.2649(4) 0.0366(9) Uani 1 1 d . . .
H14 H -0.1893 0.2719 0.2996 0.044 Uiso 1 1 calc R . .
C15 C -0.1164(5) 0.2863(2) 0.1459(4) 0.0440(10) Uani 1 1 d . . .
H15 H -0.1527 0.2492 0.1007 0.053 Uiso 1 1 calc R . .
C16 C -0.0402(4) 0.3288(2) 0.0977(4) 0.0380(9) Uani 1 1 d . . .
H16 H -0.0259 0.3200 0.0184 0.046 Uiso 1 1 calc R . .
C17 C 0.0173(3) 0.38524(18) 0.1629(3) 0.0246(7) Uani 1 1 d . . .
C18 C 0.0917(3) 0.42623(18) 0.0968(3) 0.0251(7) Uani 1 1 d . . .
H18 H 0.0907 0.4133 0.0147 0.030 Uiso 1 1 calc R . .
N19 N 0.1583(3) 0.47774(15) 0.1372(2) 0.0230(6) Uani 1 1 d . . .
C20 C 0.2234(4) 0.5097(2) 0.0492(3) 0.0321(8) Uani 1 1 d . . .
H20A H 0.1744 0.5489 0.0157 0.038 Uiso 1 1 calc R . .
H20B H 0.2212 0.4806 -0.0217 0.038 Uiso 1 1 calc R . .
C22 C 0.3801(4) 0.58786(19) 0.1967(3) 0.0301(8) Uani 1 1 d . . .
H22A H 0.4702 0.6045 0.2131 0.036 Uiso 1 1 calc R . .
H22B H 0.3208 0.6216 0.1516 0.036 Uiso 1 1 calc R . .
C24 C 0.3433(4) 0.63791(19) 0.3846(4) 0.0343(8) Uani 1 1 d . . .
H24A H 0.4261 0.6606 0.3955 0.051 Uiso 1 1 calc R . .
H24B H 0.3274 0.6299 0.4663 0.051 Uiso 1 1 calc R . .
H24C H 0.2726 0.6641 0.3341 0.051 Uiso 1 1 calc R . .
C42 C -0.0334(3) 0.60613(16) 0.2969(3) 0.0210(6) Uani 1 1 d . . .
C44 C -0.1192(4) 0.66049(19) 0.2253(3) 0.0318(8) Uani 1 1 d . . .
H64A H -0.0766 0.6797 0.1658 0.048 Uiso 1 1 calc R . .
H64B H -0.1318 0.6932 0.2844 0.048 Uiso 1 1 calc R . .
H64C H -0.2039 0.6431 0.1803 0.048 Uiso 1 1 calc R . .
O100 O 0.3259(2) 0.43190(12) 0.3680(2) 0.0216(5) Uani 1 1 d D . .
H2 H 0.408(2) 0.4428(19) 0.392(4) 0.026 Uiso 1 1 d D . .
H1 H 0.316(4) 0.4084(17) 0.431(3) 0.026 Uiso 1 1 d D . .
O31 O 0.1970(2) 0.52560(12) 0.51453(19) 0.0193(4) Uani 1 1 d . . .
O33 O 0.4161(2) 0.52548(14) 0.5908(2) 0.0297(6) Uani 1 1 d . . .
O11 O 0.0395(2) 0.45372(11) 0.3451(2) 0.0199(4) Uani 1 1 d . . .
O41 O 0.0614(2) 0.58682(12) 0.2558(2) 0.0254(5) Uani 1 1 d . . .
O43 O -0.0644(2) 0.58347(11) 0.3940(2) 0.0211(5) Uani 1 1 d . . .
C51 C 0.5311(15) 0.6731(8) 0.7896(14) 0.086(4) Uiso 0.50 1 d P . .
H51A H 0.6173 0.6580 0.7830 0.103 Uiso 0.50 1 calc PR . .
H51B H 0.4674 0.6428 0.7389 0.103 Uiso 0.50 1 calc PR . .
Cl52 Cl 0.5307(5) 0.6549(2) 0.9416(4) 0.1088(15) Uani 0.50 1 d P . .
Cl53 Cl 0.5102(5) 0.7314(3) 0.7172(4) 0.1075(14) Uani 0.50 1 d P . .
O51 O 0.2764(3) 0.35764(14) 0.5513(3) 0.0375(7) Uani 1 1 d . . .
H51 H 0.2098 0.3761 0.5606 0.045 Uiso 1 1 calc R . .
C52 C 0.2405(5) 0.2955(2) 0.4926(5) 0.0517(12) Uani 1 1 d . . .
H52A H 0.3184 0.2739 0.4812 0.062 Uiso 1 1 calc R . .
H52B H 0.1782 0.3015 0.4113 0.062 Uiso 1 1 calc R . .
H52C H 0.2007 0.2692 0.5458 0.062 Uiso 1 1 calc R . .
Ni1 Ni 0.0000 0.5000 0.5000 0.01673(13) Uani 1 2 d S . .
Ni2 Ni 0.19049(4) 0.51098(2) 0.31972(4) 0.01803(11) Uani 1 1 d . . .
N23 N 0.3491(3) 0.57501(14) 0.3197(3) 0.0216(5) Uani 1 1 d . . .
H23 H 0.4225 0.5546 0.3681 0.026 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'
Cl Cl 0.1484 0.1585 '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
C22 C21 C20 113.2(3) . . ?
O33 C32 O31 122.7(3) . . ?
O33 C32 C34 118.5(3) . . ?
O31 C32 C34 118.8(3) . . ?
O11 C12 C13 120.5(3) . . ?
O11 C12 C17 121.8(3) . . ?
C13 C12 C17 117.7(3) . . ?
C14 C13 C12 121.6(3) . . ?
C13 C14 C15 120.6(4) . . ?
C16 C15 C14 118.3(4) . . ?
C15 C16 C17 122.8(4) . . ?
C16 C17 C12 119.0(3) . . ?
C16 C17 C18 115.9(3) . . ?
C12 C17 C18 125.0(3) . . ?
N19 C18 C17 128.2(3) . . ?
C18 N19 C20 116.5(3) . . ?
C18 N19 Ni2 123.2(2) . . ?
C20 N19 Ni2 120.0(2) . . ?
N19 C20 C21 112.5(3) . . ?
N23 C22 C21 113.5(3) . . ?
O41 C42 O43 125.3(3) . . ?
O41 C42 C44 117.7(3) . . ?
O43 C42 C44 116.9(3) . . ?
C32 O31 Ni1 132.1(2) . . ?
C32 O31 Ni2 124.69(19) . . ?
Ni1 O31 Ni2 96.49(8) . . ?
C12 O11 Ni2 126.86(19) . . ?
C12 O11 Ni1 133.05(19) . . ?
Ni2 O11 Ni1 99.90(9) . . ?
C42 O41 Ni2 128.8(2) . . ?
C42 O43 Ni1 130.4(2) . . ?
Cl53 C51 Cl52 133.6(11) . . ?
O11 Ni2 N19 90.16(10) . . ?
O11 Ni2 O41 91.07(9) . . ?
N19 Ni2 O41 89.65(10) . . ?
O11 Ni2 N23 171.91(10) . . ?
N19 Ni2 N23 97.92(11) . . ?
O41 Ni2 N23 88.63(10) . . ?
O11 Ni2 O100 90.91(9) . . ?
N19 Ni2 O100 85.31(10) . . ?
O41 Ni2 O100 174.59(9) . . ?
N23 Ni2 O100 90.11(10) . . ?
O11 Ni2 O31 76.77(8) . . ?
N19 Ni2 O31 166.31(10) . . ?
O41 Ni2 O31 94.61(9) . . ?
N23 Ni2 O31 95.19(10) . . ?
O100 Ni2 O31 90.74(9) . . ?
C24 N23 C22 108.9(3) . . ?
C24 N23 Ni2 114.3(2) . . ?
C22 N23 Ni2 117.7(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
C21 C22 1.513(5) . ?
C21 C20 1.527(5) . ?
C32 O33 1.241(4) . ?
C32 O31 1.288(4) . ?
C32 C34 1.509(4) . ?
C12 O11 1.317(4) . ?
C12 C13 1.412(5) . ?
C12 C17 1.418(4) . ?
C13 C14 1.382(5) . ?
C14 C15 1.402(6) . ?
C15 C16 1.370(6) . ?
C16 C17 1.405(5) . ?
C17 C18 1.453(5) . ?
C18 N19 1.275(5) . ?
N19 C20 1.464(4) . ?
N19 Ni2 2.043(3) . ?
C22 N23 1.480(4) . ?
C24 N23 1.476(5) . ?
C42 O41 1.250(4) . ?
C42 O43 1.270(4) . ?
C42 C44 1.511(5) . ?
O100 Ni2 2.121(2) . ?
O31 Ni1 2.085(2) . ?
O31 Ni2 2.125(2) . ?
O11 Ni2 2.037(2) . ?
O11 Ni1 2.065(2) . ?
O41 Ni2 2.053(2) . ?
O43 Ni1 2.072(2) . ?
C51 Cl53 1.414(15) . ?
C51 Cl52 1.697(15) . ?
O51 C52 1.429(6) . ?
Ni1 O11 2.065(2) 3_566 ?
Ni1 O43 2.072(2) 3_566 ?
Ni1 O31 2.085(2) 3_566 ?
Ni2 N23 2.110(3) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139126721
