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_7716502
_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
'C15 H32 Br Cu N7, 1.873(Br), 0.873(H2 O), 0.127(Cl O4)'
_chemical_formula_sum            'C15 H33.75 Br2.87 Cl0.13 Cu N7 O1.38'
_chemical_formula_weight         631.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-02-08
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-08 deposited with the CCDC.	2024-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.263(4)
_cell_length_b                   14.560(4)
_cell_length_c                   21.837(6)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.548
_cell_measurement_theta_min      2.208
_cell_volume                     4535(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Venture D2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1048
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            110405
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.298
_diffrn_reflns_theta_min         2.349
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    6.063
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0795 before and 0.0584 after correction.
The Ratio of minimum to maximum transmission is 0.8189.
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    1.851
_exptl_crystal_description       block
_exptl_crystal_F_000             2524
_exptl_crystal_recrystallization_method 'vapor difussion'
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.324
_refine_diff_density_min         -1.220
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         10964
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0208P)^2^+11.4280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6588
_reflns_number_total             10964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01236d2.cif
_cod_data_source_block           mo_ib1_0m
_cod_depositor_comments
'Adding full bibliography for 7716501--7716502.cif.'
_cod_database_code               7716502
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.659
_shelx_estimated_absorpt_t_min   0.374
_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 O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(Cl1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=1-FVAR(1)
 Sof(Br3)=Sof(O1)=Sof(H1A)=Sof(H1B)=FVAR(1)
4.a Free rotating group:
 O1(H1A,H1B)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C3(H3A,H3B), C4(H4A,H4B),
 C5(H5C,H5D), C6(H6C,H6D)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_shelx_res_checksum              86952
_shelx_hkl_checksum              43280
_olex2_submission_original_sample_id ib1
_olex2_submission_special_instructions 'No special instructions were received'