Unveiling the reaction mechanism of novel copper N-alkylated tetra-azacyclophanes with outstanding superoxide dismutase activity.
Martínez-Camarena, Álvaro; Sánchez-Murcia, Pedro A; Blasco, Salvador; González, Leticia; García-España, Enrique; Chemical communications (Cambridge, England) 56 (2020) 7511–7514; doi:10.1039/d0cc01926g

data_1558135
_publ_section_title
;
 Unveiling the reaction mechanism of novel copper N-alkylated
 tetra-azacyclophanes with outstanding superoxide dismutase activity.
;
_journal_issue                   54
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7511
_journal_page_last               7514
_journal_paper_doi               10.1039/d0cc01926g
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C18 H32 Cu N7, Cl O4'
_chemical_formula_sum            'C18 H32 Cl Cu N7 O4'
_chemical_formula_weight         509.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-01-21
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-10 deposited with the CCDC.	2020-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.902(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.682(2)
_cell_length_b                   18.886(6)
_cell_length_c                   24.789(7)
_cell_measurement_reflns_used    9702
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      36.327
_cell_measurement_theta_min      2.400
_cell_volume                     4465(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0365
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            118824
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.354
_diffrn_reflns_theta_min         2.392
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.138
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1241 before and 0.0620 after correction.
The Ratio of minimum to maximum transmission is 0.8702.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       plate
_exptl_crystal_F_000             2136
_exptl_crystal_recrystallization_method 'Slow solvent evaporation'
_exptl_crystal_size_max          0.456
_exptl_crystal_size_mid          0.294
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.074(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         21612
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0295P)^2^+1.2167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0648
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                19659
_reflns_number_total             21612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01926g2.cif
_cod_data_source_block           am6_0ma
_cod_depositor_comments          'Adding full bibliography for 1558135.cif.'
_cod_database_code               1558135
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.625
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.926(5)
 0.074(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid bond restraints
 Cl2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Idealised Me refined with riding coordinates:
 C30(H30A,H30B,H30C)
;
_shelx_res_checksum              14693
_olex2_date_sample_completion    2020-01-19
_olex2_date_sample_data_collection 2020-01-19
_olex2_date_sample_submission    2020-01-17
_olex2_submission_original_sample_id am5
_olex2_submission_special_instructions 'No special instructions were received'