Tailor-made isostructural copper(ii) and nickel(ii) complexes with a newly designed (N,N)-donor scaffold as functional mimics of alkaline phosphatase
Kundu, Subhankar; Saha, Subhajit; Panda, Subhra Jyoti; Purohit, Chandra Shekhar; Biswas, Bhaskar; New Journal of Chemistry 47 (2023) 5894–5902; doi:10.1039/D2NJ06127A

data_7062300
_publ_section_title
;
 Tailor-made isostructural copper(ii) and nickel(ii) complexes with a
 newly designed (N,N)-donor scaffold as functional mimics of alkaline
 phosphatase
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5894
_journal_page_last               5902
_journal_paper_doi               10.1039/D2NJ06127A
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C13 H14 N4 Ni O, 0.5(C H4 O)'
_chemical_formula_sum            'C13.5 H16 N4 Ni O1.5'
_chemical_formula_weight         317.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-12-14 deposited with the CCDC.	2023-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                94.616(3)
_cell_angle_beta                 108.689(3)
_cell_angle_gamma                104.652(3)
_cell_formula_units_Z            4
_cell_length_a                   9.6002(3)
_cell_length_b                   11.8988(4)
_cell_length_c                   13.1563(4)
_cell_measurement_reflns_used    11205
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.1080
_cell_measurement_theta_min      3.4890
_cell_volume                     1355.75(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9967
_diffrn_measured_fraction_theta_max 0.8021
_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    -15.00  41.00   0.50    3.00    --    3.51-101.00 168.00  112
  2  \w    -15.00  33.00   0.50    3.00    --   -4.14-101.00 168.00   96
  3  \w      0.00  70.00   0.50    3.00    --    3.51  37.00 -60.00  140
  4  \w    -42.00  27.00   0.50    3.00    --    3.51 -77.00 120.00  138
  5  \w    -36.00  -5.00   0.50    3.00    --    3.51 -77.00 -30.00   62
  6  \w     -7.00  58.00   0.50    3.00    --    3.51  57.00 -90.00  130
  7  \w    -26.00  12.00   0.50    3.00    --   -4.14 -77.00  90.00   76
  8  \w    -10.00  19.00   0.50    3.00    --   -4.14 -99.00 -90.00   58
  9  \w    -14.00  13.00   0.50    3.00    --   -4.14  77.00  60.00   54
 10  \w    -40.00  19.00   0.50    3.00    --   -4.14 -77.00 -30.00  118
 11  \w     -6.00  50.00   0.50    3.00    --   -4.14  37.00 -90.00  112
 12  \w    -22.00   4.00   0.50    3.00    --   -4.14  77.00 -30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0114752000
_diffrn_orient_matrix_UB_12      -0.0334583000
_diffrn_orient_matrix_UB_13      -0.0420928000
_diffrn_orient_matrix_UB_21      -0.0749574000
_diffrn_orient_matrix_UB_22      -0.0039704000
_diffrn_orient_matrix_UB_23      -0.0356710000
_diffrn_orient_matrix_UB_31      0.0302327000
_diffrn_orient_matrix_UB_32      0.0527533000
_diffrn_orient_matrix_UB_33      -0.0172888000
_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  0.0598
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.801
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24462
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.801
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.480
_diffrn_reflns_theta_min         3.321
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.435
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark pink'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       plank
_exptl_crystal_F_000             660
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         6616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0402P)^2^+0.2715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5089
_reflns_number_total             6616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj06127a2.cif
_cod_data_source_block           csp-ni-sk-02
_cod_depositor_comments
;
Adding full bibliography for 7062300--7062301.cif.

2025-01-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C27 H32 N8 Ni2 O3'
_cod_original_formula_weight         634.02
_cod_original_formula_moiety         '2(C13 H14 N4 Ni O), C H4 O'
_cod_original_formula_units_Z            2
_cod_database_code               7062300
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C54 H66 N16 Ni4 O6 '
_chemical_oxdiff_usercomment     'DARK PINK CUBOID'
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.698
_diffrn_oxdiff_digest_frames
;
01b8b549f67ba7851dbe397dacfc18e7e401148149e
;
_diffrn_oxdiff_digest_hkl
;
01549ae8b597d021b2ca5bfd36049be12bc0ba
;
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C11(H11), C29(H29)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C30(H30A,H30B), C10(H10A,H10B), C28(H28A,H28B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C14(H14), C25(H25), C26(H26), C32(H32), C38(H38), C36(H36), C20(H20),
 C24(H24), C19(H19), C37(H37), C5(H5), C23(H23), C7(H7), C18(H18), C6(H6)
2.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C)
2.e Idealised tetrahedral OH refined as rotating group:
 O15(H15), O33(H33), O39(H39)
;
_shelx_res_checksum              3528
_olex2_exptl_crystal_mounting_method 'Mounted on the loop'
_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 1.373
_oxdiff_exptl_absorpt_empirical_full_min 0.657