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_7062301
_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 Cu N4 O'
_chemical_formula_sum            'C13 H14 Cu N4 O'
_chemical_formula_weight         305.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-12-14 deposited with the CCDC.	2023-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.669(3)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   16.3850(5)
_cell_length_b                   18.8935(7)
_cell_length_c                   18.0821(7)
_cell_measurement_reflns_used    8126
_cell_measurement_temperature    298.0(2)
_cell_measurement_theta_max      31.3440
_cell_measurement_theta_min      2.7080
_cell_volume                     5591.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_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    -69.00 118.20   0.30   30.00    --   29.89  54.00-180.00  624
  2  \w    -69.00 118.20   0.30   30.00    --   29.89  54.00 150.00  624
  3  \w    -69.00  -3.90   0.30   30.00    --   29.89  54.00 -90.00  217
  4  \w    -69.00 118.20   0.30   30.00    --   29.89  54.00   0.00  624
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0157617000
_diffrn_orient_matrix_UB_12      -0.0144547000
_diffrn_orient_matrix_UB_13      0.0339558000
_diffrn_orient_matrix_UB_21      0.0020623000
_diffrn_orient_matrix_UB_22      0.0344389000
_diffrn_orient_matrix_UB_23      0.0156043000
_diffrn_orient_matrix_UB_31      -0.0402899000
_diffrn_orient_matrix_UB_32      -0.0038622000
_diffrn_orient_matrix_UB_33      0.0121157000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            68110
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.489
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       plate
_exptl_crystal_F_000             2516
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         12794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0692P)^2^+2.3441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1573
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7820
_reflns_number_total             12794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj06127a2.cif
_cod_data_source_block           cucl2sk02dcmmeoh_rt
_cod_depositor_comments
;
Adding full bibliography for 7062300--7062301.cif.

2024-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C52 H57 Cu4 N16 O4'
_cod_original_formula_weight         1224.29
_cod_original_formula_moiety         '3(C13 H14 Cu N4 O), C13 H15 Cu N4 O'
_cod_original_formula_units_Z            4
_cod_database_code               7062301
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.746
_shelx_estimated_absorpt_t_min   0.574
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H1 of O1, H3 of O3, All C(H,H) groups
 At 1.5 times of:
  H2 of O2, H4 of O4
2.a Rotating group:
 O3(H3)
2.b Ternary CH refined with riding coordinates:
 C28(H28), C7(H7), C15(H15), C51(H51)
2.c Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C29(H29A,H29B), C0AA(H0AA,H0AB), C52(H52A,H52B), C14(H14A,
 H14B), C16(H16A,H16B), C50(H50A,H50B), C19(H19A,H19B), C8(H8A,H8B)
2.d Aromatic/amide H refined with riding coordinates:
 C30(H30), C26(H26), C39(H39), C17(H17), C49(H49), C44(H44), C46(H46),
 C34(H34), C32(H32), C45(H45), C40(H40), C47(H47), C33(H33), C21(H21), C24(H24),
  C43(H43), C23(H23), C22(H22), C35(H35), C1AA(H1AA), C9(H9), C37(H37),
 C42(H42), C36(H36), C1(H1A), C13(H13), C2(H2A), C12(H12), C11(H11), C3(H3A)
2.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.294
_oxdiff_exptl_absorpt_empirical_full_min 0.807