Exploring the carbonic anhydrase-mimetic [(PMDTA)<sub>2</sub>ZnII2(OH<sup>-</sup>)<sub>2</sub>]<sup>2+</sup> for nitric oxide monooxygenation.
Das, Sandip; Kumar, Pankaj; Dalton transactions (Cambridge, England : 2003) 53 (2024) 6173–6177; doi:10.1039/d4dt00407h

data_7715429
_publ_section_title
;
 Exploring the carbonic anhydrase-mimetic
 [(PMDTA)<sub>2</sub>ZnII2(OH<sup>-</sup>)<sub>2</sub>]<sup>2+</sup> for
 nitric oxide monooxygenation.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6173
_journal_page_last               6177
_journal_paper_doi               10.1039/d4dt00407h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C18 H46.5 N6.75 O3 Zn2, 2(C24 H20 B), C2 H3 N, 0.25(H2 O)'
_chemical_formula_sum            'C68 H90 B2 N7.75 O3.25 Zn2'
_chemical_formula_weight         1220.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-03-08 deposited with the CCDC.	2024-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.764(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7304(6)
_cell_length_b                   18.0171(7)
_cell_length_c                   26.2207(11)
_cell_measurement_reflns_used    9329
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      27.779
_cell_measurement_theta_min      2.392
_cell_volume                     6453.7(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Apex 4 using Bruker Photon III Duo'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Photon III Duo'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            266499
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.304
_diffrn_reflns_theta_min         2.084
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0798 before and 0.0560 after correction.
The Ratio of minimum to maximum transmission is 0.9287.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       Block
_exptl_crystal_F_000             2593
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.254
_refine_diff_density_max         1.605
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     980
_refine_ls_number_reflns         15979
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+7.4578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1487
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13473
_reflns_number_total             15979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00407h2.cif
_cod_data_source_block           mo_zn_p_no2_koh_bph4_0m_a
_cod_depositor_comments
'Adding full bibliography for 7715427--7715429.cif.'
_cod_database_code               7715429
_shelx_shelxl_version_number     2019/1
_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 C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N7-C10 \\sim N7-C73
 with sigma of 0.02
 N7-C11 \\sim N7-C0
 with sigma of 0.04
 N6-C11 \\sim N6-C0
 with sigma of 0.02
 C10-C11 \\sim C73-C0
 with sigma of 0.02
 N6-C10 \\sim N6-C73
 with sigma of 0.04
 C12-C0 \\sim C74-C0
 with sigma of 0.02
 N6-C13 \\sim N6-C69
 with sigma of 0.04
 N5-C13 \\sim N5-C69
 with sigma of 0.02
 N5-C12 \\sim N5-C74
 with sigma of 0.04
 N6-C12 \\sim N6-C74
 with sigma of 0.02
 C13-C0 \\sim C69-C0
 with sigma of 0.04
 C13-C12 \\sim C69-C74
 with sigma of 0.02
 N7-C10 \\sim N5A-C10
 with sigma of 0.02
 C15-C14 \\sim C15-C75
 with sigma of 0.04
 N7-C15 \\sim N5A-C15
 with sigma of 0.02
 Zn2-C14 \\sim Zn2-C75
 with sigma of 0.04
 N7-C14 \\sim N5A-C75
 with sigma of 0.02
 C10-C14 \\sim C10-C75
 with sigma of 0.04
 N7-C73 \\sim N5A-C73
 with sigma of 0.02
 C14-C73 \\sim C75-C73
 with sigma of 0.04
 Zn2-N7 \\sim Zn2-N5A
 with sigma of 0.02
 N2B-C1 \\sim N2B-C6A
 with sigma of 0.02
 N3-C1 \\sim N3-C6A
 with sigma of 0.04
 N3-C2 \\sim N3-C72
 with sigma of 0.02
 C2-C1 \\sim C72-C6A
 with sigma of 0.02
 N3-C4 \\sim N3-C02C
 with sigma of 0.04
 N4-C3 \\sim N4-C01W
 with sigma of 0.04
 N3-C3 \\sim N3-C01W
 with sigma of 0.02
 N2B-C2 \\sim N2B-C72
 with sigma of 0.04
 N4-C4 \\sim N4-C02C
 with sigma of 0.02
 C3-C4 \\sim C01W-C02C
 with sigma of 0.02
 C40-C42 \\sim C17A-C19A
 with sigma of 0.04
 C43-C44 \\sim C20A-C21A
 with sigma of 0.02
 C40-C44 \\sim C17A-C21A
 with sigma of 0.04
 C39-C43 \\sim C00{-C20A
 with sigma of 0.04
 C39-C41 \\sim C00{-C18A
 with sigma of 0.04
 B2-C44 \\sim B2-C21A
 with sigma of 0.04
 C40-B2 \\sim C17A-B2
 with sigma of 0.04
 C39-C40 \\sim C00{-C17A
 with sigma of 0.02
 C39-B2 \\sim C00{-B2
 with sigma of 0.02
 C39-C44 \\sim C00{-C21A
 with sigma of 0.02
 C41-C43 \\sim C18A-C20A
 with sigma of 0.04
 C42-C44 \\sim C19A-C21A
 with sigma of 0.04
 C40-C41 \\sim C17A-C18A
 with sigma of 0.02
 C41-C42 \\sim C18A-C19A
 with sigma of 0.02
 C42-C43 \\sim C19A-C20A
 with sigma of 0.02
 Zn1-O2 \\sim Zn1-O1A
 with sigma of 0.02
 Zn2-O3 \\sim Zn2-O3A
 with sigma of 0.02
 O3-N1 \\sim O3A-N1
 with sigma of 0.02
 N1-O2 \\sim N1-O1A
 with sigma of 0.02
 Zn2-H3AA \\sim Zn2-H3AB
 with sigma of 0.02
3. Rigid bond restraints
 O3A, O3, N1, O2, O1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O3A \\sim O3 \\sim O2 \\sim O1A \\sim N1: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(O3A) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(O1A)
\\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(O2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C75) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C21A)=Sof(H21A)=Sof(C00{)=Sof(C17A)=Sof(H17D)=Sof(C18A)=Sof(H18D)=
 Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=1-FVAR(1)
 Sof(C39)=Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42)=Sof(C43)=
 Sof(H43)=Sof(C44)=Sof(H44)=FVAR(1)
 Fixed Sof: O3(0.75) N7(0.5) N2B(0.5) C6B(0.5) H6BA(0.5) H6BB(0.5) H6BC(0.5)
 C13(0.5) H13A(0.5) H13B(0.5) C12(0.5) H12A(0.5) H12B(0.5) C3(0.5) H3A(0.5)
 H3B(0.5) C10(0.5) H10A(0.5) H10B(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5)
 H15D(0.5) H15E(0.5) H15F(0.5) H15A(0.5) H15B(0.5) H15C(0.5) H17A(0.5)
 H17B(0.5) H17C(0.5) C11(0.5) H11A(0.5) H11B(0.5) C2(0.5) H2A(0.5) H2B(0.5)
 C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
 C5B(0.5) H5BA(0.5) H5BB(0.5) H5BC(0.5) C4(0.5) H4A(0.5) H4B(0.5) C0(0.5)
 H0A(0.5) H0B(0.5) C73(0.5) H73A(0.5) H73B(0.5) C69(0.5) H69A(0.5) H69B(0.5)
 C74(0.5) H74A(0.5) H74B(0.5) C75(0.5) H75A(0.5) H75B(0.5) H75C(0.5) N5A(0.5)
 C1(0.5) H1A(0.5) H1B(0.5) C02C(0.5) H02A(0.5) H02B(0.5) C01W(0.5) H01A(0.5)
 H01B(0.5) C72(0.5) H72A(0.5) H72B(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5) C70(0.5)
 H70A(0.5) H70B(0.5) H70C(0.5) C71(0.5) H71A(0.5) H71B(0.5) H71C(0.5) N1(0.75)
 O2(0.75) O3A(0.25) H3AA(0.25) H3AB(0.25) O1A(0.25) H1AA(0.25) H1AB(0.25)
 O2A(0.25) H2AA(0.25) H2AB(0.25) C5A(0.5) H5AA(0.5) H5AB(0.5) H5AC(0.5) N2(0.5)
 C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
6.a Riding coordinates:
 O3A(H3AA,H3AB), O1A(H1AA,H1AB), O2A(H2AA,H2AB)
6.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C12(H12A,H12B), C3(H3A,H3B), C10(H10A,H10B), C11(H11A,H11B),
 C2(H2A,H2B), C4(H4A,H4B), C0(H0A,H0B), C73(H73A,H73B), C69(H69A,H69B),
 C74(H74A,H74B), C1(H1A,H1B), C02C(H02A,H02B), C01W(H01A,H01B), C72(H72A,H72B),
 C6A(H6AA,H6AB)
6.c Me refined with riding coordinates:
 C6B(H6BA,H6BB,H6BC), C17(H17A,H17B,H17C), C5B(H5BA,H5BB,H5BC), C5A(H5AA,H5AB,
 H5AC), C5(H5A,H5B,H5C)
6.d Aromatic/amide H refined with riding coordinates:
 C62(H62), C58(H58), C56(H56), C61(H61), C60(H60), C52(H52), C32(H32),
 C31(H31), C38(H38), C46(H46), C59(H59), C29(H29), C28(H28), C25(H25), C36(H36),
  C55(H55), C26(H26), C47(H47), C24(H24), C64(H64), C40(H40), C68(H68),
 C41(H41), C48(H48), C42(H42), C50(H50), C43(H43), C22(H22), C34(H34), C37(H37),
  C54(H54), C66(H66), C67(H67), C53(H53), C35(H35), C65(H65), C49(H49),
 C23(H23), C44(H44), C30(H30), C21A(H21A), C17A(H17D), C18A(H18D), C19A(H19A),
 C20A(H20A)
6.e Idealised Me refined as rotating group:
 C19(H19B,H19C,H19D), C16(H16A,H16B,H16C), C7(H7A,H7B,H7C), C18(H18A,H18B,
 H18C), C8(H8A,H8B,H8C), C15(H15D,H15E,H15F), C15(H15A,H15B,H15C), C9(H9A,H9B,
 H9C), C14(H14A,H14B,H14C), C75(H75A,H75B,H75C), C70(H70A,H70B,H70C), C71(H71A,
 H71B,H71C)
;
_shelx_res_checksum              68291
_olex2_submission_special_instructions 'No special instructions were received'