#------------------------------------------------------------------------------
#$Date: 2025-07-06 20:04:03 +0300 (Sun, 06 Jul 2025) $
#$Revision: 300965 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/80/7718063.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_7718063
loop_
_publ_author_name
'de Campos, Élvio Antônio'
'Silva, Luana Thayline Casagrande'
'Rodrigues, Rodrigo Vieira'
'de Souza, Ronan Farias Freire'
'Dos Santos, Jeane Patrícia Cardozo'
'Olguin, Conceição de Fátima Alves'
'Buzanello, Cleide Viviane'
'Ellena, Javier Alcides'
'Santiago, Pedro Henrique de Oliveira'
'Denofre de Campos, Sílvia'
_publ_section_title
;
 A nickel glutamate metal biomolecule framework.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4645
_journal_page_last               4655
_journal_paper_doi               10.1039/d4dt03413a
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C5 H9 N Ni O5, H2 O'
_chemical_formula_sum            'C5 H11 N Ni O6'
_chemical_formula_weight         239.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-02
_audit_creation_method
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-04-17 deposited with the CCDC.	2025-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0577(2)
_cell_length_b                   10.2307(3)
_cell_length_c                   11.5950(4)
_cell_measurement_reflns_used    5177
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.9240
_cell_measurement_theta_min      2.6440
_cell_volume                     837.22(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00   9.00   0.50    3.00    --  -12.12 -77.00 -90.00   50
  2  ω    -16.00  10.00   0.50    3.00    --  -12.12 -77.00-180.00   52
  3  ω    -27.00   0.00   0.50    3.00    --  -12.12 -57.00 -90.00   54
  4  ω     -9.00  44.00   0.50    3.00    --  -12.12  20.00 107.00  106
  5  ω      5.00  36.00   0.50    3.00    --   12.91  57.00  30.00   62
  6  ω    -52.00 -27.00   0.50    3.00    --   12.91 -19.00 -90.00   50
  7  ω    -60.00 -35.00   0.50    3.00    --   12.91 -20.00 -59.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0247351000
_diffrn_orient_matrix_UB_12      -0.0583811000
_diffrn_orient_matrix_UB_13      0.0293452000
_diffrn_orient_matrix_UB_21      0.0111766000
_diffrn_orient_matrix_UB_22      0.0357889000
_diffrn_orient_matrix_UB_23      0.0519519000
_diffrn_orient_matrix_UB_31      -0.0967800000
_diffrn_orient_matrix_UB_32      -0.0107828000
_diffrn_orient_matrix_UB_33      0.0134838000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5632
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.691
_diffrn_reflns_theta_min         2.655
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.317
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 762 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0190
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0198P)²+0.1786P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0438
_reflns_Friedel_coverage         0.623
_reflns_Friedel_fraction_full    0.944
_reflns_Friedel_fraction_max     0.878
_reflns_number_gt                2006
_reflns_number_total             2065
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt03413a2.cif
_cod_data_source_block           20230227ron01_auto
_cod_depositor_comments          'Adding full bibliography for 7718063.cif.'
_cod_original_cell_volume        837.23(5)
_cod_database_code               7718063
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C15 H29 N3 O13 Ni'
_chemical_oxdiff_usercomment
'Ronan Farias Freire de Souza - Amostra 1 -27-02-2023'
_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_max   0.820
_shelx_estimated_absorpt_t_min   0.733
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O6(H6A,H6B)
2.b Rotating group:
 O5(H5A,H5B)
2.c Ternary CH refined with riding coordinates:
 C2(H2)
2.d Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B)
;
_olex2_date_sample_data_collection 2023-02-27
_olex2_date_sample_submission    2023-02-17
_olex2_submission_original_sample_id 'Amostra 01'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.341
_oxdiff_exptl_absorpt_empirical_full_min 0.781
loop_
_space_group_symop_operation_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'
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
Ni1 Ni 0.86425(3) 0.55722(3) 0.95993(2) 0.00654(8) Uani 1 1 d . . . . .
O2 O 0.5184(2) 0.77534(16) 1.01996(14) 0.0093(3) Uani 1 1 d . . . . .
O3 O 0.88846(19) 0.93835(16) 0.52941(13) 0.0101(3) Uani 1 1 d . . . . .
O4 O 0.9894(2) 1.00799(16) 0.69724(15) 0.0112(3) Uani 1 1 d . . . . .
O5 O 0.7161(2) 0.38390(15) 0.94358(15) 0.0105(3) Uani 1 1 d . . . . .
H5A H 0.640585 0.373273 1.003261 0.016 Uiso 1 1 d R U . . .
H5B H 0.794464 0.317153 0.947890 0.016 Uiso 1 1 d R U . . .
O1 O 0.6449(2) 0.64845(14) 0.88291(13) 0.0087(3) Uani 1 1 d . . . . .
O6 O 0.5818(2) 0.85509(16) 0.40569(15) 0.0119(3) Uani 1 1 d G . . . .
H6A H 0.674608 0.896135 0.439224 0.018 Uiso 1 1 d G U . . .
H6B H 0.561103 0.889436 0.338202 0.018 Uiso 1 1 d G U . . .
N1 N 0.2918(3) 0.89938(19) 0.87243(18) 0.0074(4) Uani 1 1 d . . . . .
C1 C 0.5427(3) 0.7417(2) 0.9162(2) 0.0075(4) Uani 1 1 d . . . . .
C3 C 0.5920(3) 0.9146(2) 0.7673(2) 0.0088(4) Uani 1 1 d . . . . .
H3A H 0.525104 0.976533 0.715832 0.011 Uiso 1 1 calc R U . . .
H3B H 0.653473 0.966017 0.829186 0.011 Uiso 1 1 calc R U . . .
C5 C 0.8787(3) 0.9357(2) 0.63863(19) 0.0087(4) Uani 1 1 d . . . . .
C2 C 0.4473(3) 0.8214(2) 0.8213(2) 0.0068(4) Uani 1 1 d . . . . .
H2 H 0.395396 0.761533 0.760851 0.008 Uiso 1 1 calc R U . . .
C4 C 0.7444(3) 0.8431(2) 0.6982(2) 0.0118(5) Uani 1 1 d . . . . .
H4A H 0.817283 0.785745 0.750692 0.014 Uiso 1 1 calc R U . . .
H4B H 0.682627 0.787005 0.639658 0.014 Uiso 1 1 calc R U . . .
H1A H 0.258(4) 0.960(3) 0.824(2) 0.005(6) Uiso 1 1 d . . . . .
H1B H 0.189(4) 0.857(3) 0.879(3) 0.027(9) 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'
Ni Ni 0.3393 1.1124 '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'
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
O2 Ni1 O3 92.05(6) 4_567 3_746 ?
O2 Ni1 O4 92.14(6) 4_567 3_746 ?
O2 Ni1 O5 177.71(7) 4_567 . ?
O2 Ni1 N1 81.00(7) 4_567 4_567 ?
O2 Ni1 C5 94.79(7) 4_567 3_746 ?
O3 Ni1 O4 61.51(6) 3_746 3_746 ?
O3 Ni1 C5 30.78(6) 3_746 3_746 ?
O4 Ni1 C5 30.88(7) 3_746 3_746 ?
O5 Ni1 O3 85.98(6) . 3_746 ?
O5 Ni1 O4 87.95(6) . 3_746 ?
O5 Ni1 C5 84.12(7) . 3_746 ?
O1 Ni1 O2 94.09(6) . 4_567 ?
O1 Ni1 O3 156.75(6) . 3_746 ?
O1 Ni1 O4 95.83(6) . 3_746 ?
O1 Ni1 O5 88.17(6) . . ?
O1 Ni1 N1 97.34(7) . 4_567 ?
O1 Ni1 C5 126.15(7) . 3_746 ?
N1 Ni1 O3 105.77(7) 4_567 3_746 ?
N1 Ni1 O4 165.53(7) 4_567 3_746 ?
N1 Ni1 O5 98.40(7) 4_567 . ?
N1 Ni1 C5 136.50(7) 4_567 3_746 ?
C1 O2 Ni1 114.19(15) . 4_467 ?
C5 O3 Ni1 89.92(12) . 3_756 ?
C5 O4 Ni1 88.76(13) . 3_756 ?
C1 O1 Ni1 130.99(15) . . ?
C2 N1 Ni1 108.09(13) . 4_467 ?
O2 C1 C2 118.8(2) . . ?
O1 C1 O2 125.3(2) . . ?
O1 C1 C2 115.9(2) . . ?
C4 C3 C2 112.70(19) . . ?
O3 C5 Ni1 59.29(10) . 3_756 ?
O3 C5 O4 119.18(19) . . ?
O3 C5 C4 120.3(2) . . ?
O4 C5 Ni1 60.35(11) . 3_756 ?
O4 C5 C4 120.4(2) . . ?
C4 C5 Ni1 170.65(15) . 3_756 ?
N1 C2 C1 109.01(18) . . ?
N1 C2 C3 108.83(19) . . ?
C1 C2 C3 109.48(17) . . ?
C5 C4 C3 112.47(19) . . ?
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
Ni1 O2 2.0426(16) 4_567 ?
Ni1 O3 2.1309(15) 3_746 ?
Ni1 O4 2.1545(17) 3_746 ?
Ni1 O5 2.0671(15) . ?
Ni1 O1 2.0164(15) . ?
Ni1 N1 2.058(2) 4_567 ?
Ni1 C5 2.478(2) 3_746 ?
O2 C1 1.263(3) . ?
O3 C5 1.269(3) . ?
O4 C5 1.272(3) . ?
O1 C1 1.257(3) . ?
N1 C2 1.481(3) . ?
C1 C2 1.527(3) . ?
C3 C2 1.531(3) . ?
C3 C4 1.527(3) . ?
C5 C4 1.508(3) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O5 H5A O6 0.88 1.90 2.750(2) 161.6 3_646 yes
O5 H5B O6 0.88 2.03 2.864(2) 158.7 2_665 yes
O6 H6A O3 0.87 1.89 2.733(2) 163.9 . yes
O6 H6B O4 0.87 1.97 2.839(2) 171.6 2_674 yes
N1 H1A O4 0.87(3) 2.45(3) 3.149(3) 138(2) 1_455 yes
N1 H1B O2 0.85(3) 2.16(3) 2.911(3) 147(3) 4_467 yes
