A nickel glutamate metal biomolecule framework.
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; Dalton transactions (Cambridge, England : 2003) 54 (2025) 4645–4655; doi:10.1039/d4dt03413a

data_7718063
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -16.00   9.00   0.50    3.00    --  -12.12 -77.00 -90.00   50
  2  \w    -16.00  10.00   0.50    3.00    --  -12.12 -77.00-180.00   52
  3  \w    -27.00   0.00   0.50    3.00    --  -12.12 -57.00 -90.00   54
  4  \w     -9.00  44.00   0.50    3.00    --  -12.12  20.00 107.00  106
  5  \w      5.00  36.00   0.50    3.00    --   12.91  57.00  30.00   62
  6  \w    -52.00 -27.00   0.50    3.00    --   12.91 -19.00 -90.00   50
  7  \w    -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       '\w 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/[\s^2^(Fo^2^)+(0.0198P)^2^+0.1786P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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)
;
_shelx_res_checksum              20944
_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