Role of heteroatom substitution on the stability and reactivity of mononuclear Cu(II)-alkylperoxo complexes.
Sahoo, Limashree; Zhang, Yi; Das, Amrit; de Visser, Sam P.; Sastri, Chivukula V.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14367–14375; doi:10.1039/d5dt01804h

data_7719583
_publ_section_title
;
 Role of heteroatom substitution on the stability and reactivity of
 mononuclear Cu(II)-alkylperoxo complexes.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14367
_journal_page_last               14375
_journal_paper_doi               10.1039/d5dt01804h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C17 H23 Cu N4 O2, 2(Cl O4)'
_chemical_formula_sum            'C17 H23 Cl2 Cu N4 O10'
_chemical_formula_weight         577.83
_chemical_name_systematic        Cu-Ome-ClO4
_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     iterative
_audit_creation_date             2024-10-18
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-10-28 deposited with the CCDC.	2025-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.470(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0427(10)
_cell_length_b                   10.7911(10)
_cell_length_c                   15.2974(12)
_cell_measurement_reflns_used    9665
_cell_measurement_temperature    298.00
_cell_measurement_theta_max      28.65
_cell_measurement_theta_min      2.33
_cell_volume                     2424.6(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_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)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.00
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            65932
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.682
_diffrn_reflns_theta_min         2.328
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.179
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1381 before and 0.0600 after correction.
The Ratio of minimum to maximum transmission is 0.8557.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic bluish blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         6149
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1454
_refine_ls_R_factor_gt           0.0858
_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^)+(0.0946P)^2^+4.8834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1983
_refine_ls_wR_factor_ref         0.2446
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3653
_reflns_number_total             6149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01804h19.cif
_cod_data_source_block           cuomeclo4_1_0ma_a
_cod_database_code               7719583
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.912
_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 O(H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
3.a Rotating group:
 O2(H2A,H2B)
3.b Secondary CH2 refined with riding coordinates:
 C00C(H00A,H00C), C00I(H00D,H00E), C00Q(H00R,H00S)
3.c Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00F(H00F), C00H(H00H), C00K(H00K), C00L(H00L), C00O(H00P),
 C00P(H00Q), C00R(H00T), C00S(H00U)
3.d Idealised Me refined as rotating group:
 C00J(H00G,H00I,H00J), C00M(H00M,H00N,H00O)
;
_olex2_submission_original_sample_id Cu-Ome-ClO4
_olex2_submission_special_instructions 'No special instructions were received'