Exo- or endo-1<i>H</i>-pyrazole metal coordination modulated by the polyamine chain length in [1 + 1] condensation azamacrocycles. Binuclear complexes with remarkable SOD activity.
Bonastre-Sabater, Irene; Lopera, Alberto; Martínez-Camarena, Álvaro; Blasco, Salvador; Doménech-Carbó, Antonio; Jiménez, Hermas R; Verdejo, Begoña; García-España, Enrique; Clares, M. Paz; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16480–16494; doi:10.1039/d4dt01236d

data_7716501
_publ_section_title
;
 Exo- or endo-1<i>H</i>-pyrazole metal coordination modulated by the
 polyamine chain length in [1 + 1] condensation azamacrocycles. Binuclear
 complexes with remarkable SOD activity.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16480
_journal_page_last               16494
_journal_paper_doi               10.1039/d4dt01236d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C18 H37 Cl Cu2 N8, 2(Cl O4), C2 H6 O, H2 O'
_chemical_formula_sum            'C20 H45 Cl3 Cu2 N8 O10'
_chemical_formula_weight         791.07
_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   mixed
_audit_creation_date             2022-10-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-27 deposited with the CCDC.	2024-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                66.818(7)
_cell_angle_beta                 69.337(8)
_cell_angle_gamma                65.348(12)
_cell_formula_units_Z            2
_cell_length_a                   11.925(3)
_cell_length_b                   11.935(3)
_cell_length_c                   13.621(4)
_cell_measurement_reflns_used    1248
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.47
_cell_measurement_theta_min      2.82
_cell_volume                     1577.8(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.06
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40075
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.248
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.665
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0917 before and 0.0636 after correction.
The Ratio of minimum to maximum transmission is 0.7135.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.146
_refine_diff_density_max         1.701
_refine_diff_density_min         -1.476
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         5547
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1743
_refine_ls_R_factor_gt           0.1161
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+34.9993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2461
_refine_ls_wR_factor_ref         0.2925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3663
_reflns_number_total             5547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01236d2.cif
_cod_data_source_block           sb17_0m
_cod_depositor_comments
'Adding full bibliography for 7716501--7716502.cif.'
_cod_database_code               7716501
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.793
_shelx_estimated_absorpt_t_min   0.678
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 N7-C16B \\sim N7-C16A
 with sigma of 0.02
 N6-C14A \\sim N6-C14B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C14B) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C15B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Sof(H6B)=Sof(C14B)=Sof(H14A)=Sof(H14B)=Sof(H7BB)=Sof(C16B)=Sof(H16A)=
 Sof(H16B)=Sof(C15B)=Sof(H15A)=Sof(H15B)=1-FVAR(1)
 Sof(H6A)=Sof(H7AA)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15C)=
 Sof(H15D)=Sof(C16A)=Sof(H16C)=Sof(H16D)=FVAR(1)
5.a Free rotating group:
 O2(H2A,H2B)
5.b Ternary CH refined with riding coordinates:
 N2(H2), N4(H4), N3(H3), N5(H5), N6(H6B), N6(H6A), N7(H7BB), N7(H7AA)
5.c Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C9(H9A,H9B), C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C17(H17A,
 H17B), C12(H12A,H12B), C13(H13A,H13B), C6(H6C,H6D), C14B(H14A,H14B), C19(H19A,
 H19B), C4(H4A,H4B), C5(H5A,H5B), C11(H11A,H11B), C16B(H16A,H16B), C15B(H15A,
 H15B), C14A(H14C,H14D), C15A(H15C,H15D), C16A(H16C,H16D)
5.d Aromatic/amide H refined with riding coordinates:
 C1(H1)
5.e Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
5.f Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;
_shelx_res_checksum              12075
_shelx_hkl_checksum              10895
_olex2_date_sample_completion    2019-11-29
_olex2_date_sample_data_collection 2019-11-29
_olex2_date_sample_submission    2019-11-28
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MiteGen 100um micromount.'
_olex2_submission_original_sample_id sb17
_olex2_submission_special_instructions 'No special instructions were received'