#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:40:30 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301839 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/88/4338821.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_4338821
loop_
_publ_author_name
'Meier, Roland'
'Platas-Iglesias, Carlos'
'Heinemann, Frank W.'
'Linti, Gerald'
'Schulte, Jürgen'
'Srivastava, Sunil K.'
_publ_section_title
;
 Secrets of Solid State and Aqueous Solution Structures of
 [Ni(tmdta)](2-).
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6684
_journal_page_last               6697
_journal_paper_doi               10.1021/ic5004325
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C11 H14 N2 Ni O8, H10 Ni O6, 2(H2 O)'
_chemical_formula_sum            'C11 H28 N2 Ni2 O16'
_chemical_formula_weight         561.77
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      52
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_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                   13.213(3)
_cell_length_b                   11.612(2)
_cell_length_c                   13.676(3)
_cell_measurement_temperature    200(2)
_cell_volume                     2098.3(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23440
_diffrn_reflns_theta_full        30.36
_diffrn_reflns_theta_max         30.36
_diffrn_reflns_theta_min         2.77
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.876
_exptl_absorpt_correction_T_max  0.4953
_exptl_absorpt_correction_T_min  0.4040
_exptl_absorpt_correction_type   numerical
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.506
_exptl_crystal_size_mid          0.479
_exptl_crystal_size_min          0.412
_refine_diff_density_max         1.160
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0654P)²+1.3748P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                2770
_reflns_number_total             3144
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5004325_si_002.cif
_cod_data_source_block           Ni(H2O)6-Ni(tmdta)-2H2O-2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4338819--4338821.cif.
;
_cod_original_cell_volume        2098.4(7)
_cod_database_code               4338821
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-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
N1 N 0.11335(10) 0.71926(13) 0.36027(10) 0.0126(2) Uani 1 1 d .
Ni1 Ni -0.39428(2) 0.7500 0.2500 0.00946(10) Uani 1 2 d S
Ni2 Ni 0.00843(2) 0.7500 0.2500 0.01094(11) Uani 1 2 d S
C1 C 0.20802(13) 0.67045(16) 0.31954(13) 0.0200(3) Uani 1 1 d .
C2 C 0.2659(2) 0.7500 0.2500 0.0306(7) Uani 1 2 d S
C3 C 0.06214(12) 0.63520(13) 0.42466(12) 0.0154(3) Uani 1 1 d .
C4 C -0.05128(12) 0.65851(12) 0.42990(11) 0.0138(3) Uani 1 1 d .
C5 C 0.13241(14) 0.82752(14) 0.41458(13) 0.0180(3) Uani 1 1 d .
C6 C 0.07757(13) 0.93137(14) 0.37401(12) 0.0168(3) Uani 1 1 d .
O1 O -0.09836(10) 0.63142(11) 0.50525(9) 0.0200(3) Uani 1 1 d .
O2 O -0.09200(9) 0.70046(11) 0.35354(9) 0.0162(2) Uani 1 1 d .
O3 O 0.01487(9) 0.91640(10) 0.30521(9) 0.0177(2) Uani 1 1 d .
O4 O 0.09855(12) 1.02615(11) 0.41246(11) 0.0294(3) Uani 1 1 d .
O5 O -0.40305(11) 0.57966(11) 0.29154(11) 0.0232(3) Uani 1 1 d .
O6 O -0.50143(10) 0.78274(13) 0.35867(10) 0.0205(3) Uani 1 1 d .
O7 O -0.28225(10) 0.78345(13) 0.35317(10) 0.0221(3) Uani 1 1 d .
O8 O 0.2500 0.5000 0.58697(14) 0.0195(3) Uani 1 2 d S
O9 O -0.2500 1.0000 0.43949(14) 0.0223(4) Uani 1 2 d S
H3B H 0.0739(18) 0.559(2) 0.3993(18) 0.022(6) Uiso 1 1 d .
H1B H 0.1834(19) 0.596(2) 0.287(2) 0.027(6) Uiso 1 1 d .
H5B H 0.202(2) 0.846(2) 0.4162(18) 0.027(6) Uiso 1 1 d .
H5D H -0.349(2) 0.544(2) 0.3241(19) 0.029(6) Uiso 1 1 d .
H1A H 0.253(2) 0.645(2) 0.3707(18) 0.026(6) Uiso 1 1 d .
H3A H 0.0935(17) 0.6378(19) 0.4884(17) 0.014(5) Uiso 1 1 d .
H5C H -0.440(4) 0.514(5) 0.257(3) 0.098(19) Uiso 1 1 d .
H6B H -0.526(2) 0.727(3) 0.390(2) 0.028(7) Uiso 1 1 d .
H6A H -0.528(2) 0.846(3) 0.375(2) 0.035(7) Uiso 1 1 d .
H5A H 0.111(2) 0.823(3) 0.481(2) 0.032(7) Uiso 1 1 d .
H7A H -0.266(3) 0.843(3) 0.368(3) 0.057(10) Uiso 1 1 d .
H9A H -0.200(2) 0.985(3) 0.482(2) 0.048(9) Uiso 1 1 d .
H2A H 0.315(3) 0.800(4) 0.281(3) 0.058(10) Uiso 1 1 d .
H8A H 0.217(2) 0.452(3) 0.546(2) 0.034(7) Uiso 1 1 d .
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'
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
C3 N1 C5 109.84(13) . .
C3 N1 C1 110.95(13) . .
C5 N1 C1 111.68(14) . .
C3 N1 Ni2 103.90(10) . .
C5 N1 Ni2 109.34(10) . .
C1 N1 Ni2 110.85(11) . .
O5 Ni1 O5 173.55(8) 4_565 .
O5 Ni1 O7 92.74(6) 4_565 .
O5 Ni1 O7 91.85(6) . .
O5 Ni1 O7 91.85(6) 4_565 4_565
O5 Ni1 O7 92.74(6) . 4_565
O7 Ni1 O7 89.35(8) . 4_565
O5 Ni1 O6 86.59(6) 4_565 4_565
O5 Ni1 O6 89.04(6) . 4_565
O7 Ni1 O6 177.27(6) . 4_565
O7 Ni1 O6 88.03(6) 4_565 4_565
O5 Ni1 O6 89.04(6) 4_565 .
O5 Ni1 O6 86.59(6) . .
O7 Ni1 O6 88.03(6) . .
O7 Ni1 O6 177.27(6) 4_565 .
O6 Ni1 O6 94.59(8) 4_565 .
O2 Ni2 O2 98.07(7) 4_565 .
O2 Ni2 O3 92.12(5) 4_565 4_565
O2 Ni2 O3 90.96(5) . 4_565
O2 Ni2 O3 90.96(5) 4_565 .
O2 Ni2 O3 92.12(5) . .
O3 Ni2 O3 175.30(7) 4_565 .
O2 Ni2 N1 173.35(5) 4_565 .
O2 Ni2 N1 83.16(5) . .
O3 Ni2 N1 94.40(5) 4_565 .
O3 Ni2 N1 82.46(5) . .
O2 Ni2 N1 83.16(5) 4_565 4_565
O2 Ni2 N1 173.35(5) . 4_565
O3 Ni2 N1 82.46(5) 4_565 4_565
O3 Ni2 N1 94.40(5) . 4_565
N1 Ni2 N1 96.37(8) . 4_565
N1 C1 C2 115.12(15) . .
C1 C2 C1 120.0(2) 4_565 .
N1 C3 C4 111.14(12) . .
O1 C4 O2 124.44(15) . .
O1 C4 C3 119.05(14) . .
O2 C4 C3 116.44(14) . .
N1 C5 C6 114.28(14) . .
O4 C6 O3 125.35(15) . .
O4 C6 C5 116.18(15) . .
O3 C6 C5 118.48(14) . .
C4 O2 Ni2 113.96(10) . .
C6 O3 Ni2 115.15(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C3 1.479(2) .
N1 C5 1.482(2) .
N1 C1 1.482(2) .
N1 Ni2 2.0793(14) .
Ni1 O5 2.0612(13) 4_565
Ni1 O5 2.0612(13) .
Ni1 O7 2.0816(14) .
Ni1 O7 2.0816(14) 4_565
Ni1 O6 2.0876(13) 4_565
Ni1 O6 2.0876(13) .
Ni2 O2 2.0241(12) 4_565
Ni2 O2 2.0241(12) .
Ni2 O3 2.0763(12) 4_565
Ni2 O3 2.0763(13) .
Ni2 N1 2.0793(14) 4_565
C1 C2 1.531(2) .
C2 C1 1.531(2) 4_565
C3 C4 1.525(2) .
C4 O1 1.244(2) .
C4 O2 1.2717(19) .
C5 C6 1.512(2) .
C6 O4 1.251(2) .
C6 O3 1.266(2) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168338110
