Synthesis of Ni(II) and Zn(II) complexes of pyrrolyl dipyrrins and their biomimetic role in catalyzing the hydrolysis of the phospho-ester bond.
Chauhan, Pinky; Sarkar, Abani; Ravikanth, Mangalampalli; Dalton transactions (Cambridge, England : 2003) 55 (2026) 1349–1359; doi:10.1039/d5dt02700d

data_7720560
_publ_section_title
;
 Synthesis of Ni(II) and Zn(II) complexes of pyrrolyl dipyrrins and their
 biomimetic role in catalyzing the hydrolysis of the phospho-ester bond.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1349
_journal_page_last               1359
_journal_paper_doi               10.1039/d5dt02700d
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C40 H32 N6 Zn'
_chemical_formula_sum            'C40 H32 N6 Zn'
_chemical_formula_weight         662.136
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-04-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-05-16 deposited with the CCDC.	2025-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.865(1)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   32.7458(4)
_cell_length_b                   12.4657(2)
_cell_length_c                   33.4685(5)
_cell_measurement_reflns_used    27849
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.4320
_cell_measurement_theta_min      1.7520
_cell_volume                     13660.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.9984
_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   -122.88  23.12   0.50   10.00    --  -18.16 -59.25 122.08  292
  2  \f    -70.17 153.83   0.50   10.00  72.70 -18.16  31.50    --   448
  3  \w   -122.88  23.12   0.50   10.00    --  -18.16 -59.25  20.08  292
  4  \w   -122.88  23.12   0.50   10.00    --  -18.16 -59.25 173.08  292
  5  \f   -153.53  37.97   0.50   10.00  31.10 -18.16 -31.50    --   383
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.9984
_diffrn_reflns_Laue_measured_fraction_max 0.9984
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            133845
_diffrn_reflns_point_group_measured_fraction_full 0.9984
_diffrn_reflns_point_group_measured_fraction_max 0.9984
_diffrn_reflns_theta_full        24.9984
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic pinkish'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       block
_exptl_crystal_F_000             5512.393
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.4546
_refine_diff_density_min         -0.3902
_refine_diff_density_rms         0.0669
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             11.0207
_refine_ls_goodness_of_fit_ref   1.0489
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    120
_refine_ls_number_parameters     851
_refine_ls_number_reflns         12014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0489
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+24.3051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              38
_reflns_limit_h_min              -38
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              39
_reflns_limit_l_min              0
_reflns_number_gt                10697
_reflns_number_total             12014
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5dt02700d2.cif
_cod_data_source_block           mr_pc_re_autored
_cod_original_formula_sum        'C40 H32 N6 Zn1'
_cod_database_code               7720560
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), C3(H3a), C4(H4), C6(H6a), C7(H7), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24),
  C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35),
 C38(H38), C39(H39), C40(H40), N9(H9), N12(H12a), C43(H43), C44(H44), C46(H46),
 C47(H47), C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C58(H58), C59(H59),
  C60(H60), C63(H63), C64(H64), C66(H66), C67(H67), C70(H70), C71(H71),
 C72(H72), C74(H74), C75(H75), C78(H78), C79(H79), C80(H80)
2.b Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C21(H21a,H21b,H21c), C41(H41a,H41b,H41c), C61(H61a,H61b,H61c)
;
_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
- Detector area scaling
;