Tuning the reactivity of copper complexes supported by tridentate ligands leading to two-electron reduction of dioxygen.
Suktanarak, Pattira; Watchasit, Sarayut; Chitchak, Kantima; Plainpan, Nukorn; Chainok, Kittipong; Vanalabhpatana, Parichatr; Pienpinijtham, Prompong; Suksai, Chomchai; Tuntulani, Thawatchai; Ruangpornvisuti, Vithaya; Leeladee, Pannee; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16337–16349; doi:10.1039/c8dt03183e

data_7047826
_publ_section_title
;
 Tuning the reactivity of copper complexes supported by tridentate ligands
 leading to two-electron reduction of dioxygen.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16337
_journal_page_last               16349
_journal_paper_doi               10.1039/c8dt03183e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '2(C27 H23 Cl Cu N3), 2(Cl O4)'
_chemical_formula_sum            'C54 H46 Cl4 Cu2 N6 O8'
_chemical_formula_weight         1175.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-04-13 deposited with the CCDC.
2018-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.684(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.5432(11)
_cell_length_b                   12.0648(12)
_cell_length_c                   20.0110(18)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    296
_cell_measurement_theta_max      24.875
_cell_measurement_theta_min      3.094
_cell_volume                     2777.6(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.0
_diffrn_detector                 'Bruker PHOTON 100 area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'PHOTON area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_monochromator  'graphiteDouble Bounce Multilayer Mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0934
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            51374
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.436
_diffrn_reflns_theta_min         3.093
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I\mus'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.015
_exptl_absorpt_correction_T_max  0.7369
_exptl_absorpt_correction_T_min  0.6721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0987 before and 0.0849 after correction. The Ratio of minimum to maximum transmission is 0.9121. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       plate
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5692
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0587P)^2^+1.7608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1240
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4146
_reflns_number_total             5692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03183e2.cif
_cod_data_source_block           pl8
_cod_depositor_comments
'Adding full bibliography for 7047824--7047826.cif.'
_cod_database_code               7047826
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O1A-O2A \\sim O1A-O4A \\sim O1A-O3A \\sim O2A-O4A \\sim O2A-O3A \\sim O3B-O1B
\\sim O3B-O4B \\sim O3B-O2B
 \\sim O4A-O3A \\sim O1B-O4B \\sim O1B-O2B \\sim O4B-O2B
 with sigma of 0.04
 Cl2-O1A \\sim Cl2-O2A \\sim Cl2-O3B \\sim Cl2-O4A \\sim Cl2-O1B \\sim Cl2-O3A
\\sim Cl2-O4B \\sim Cl2-O2B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim O1A \\sim O2A \\sim O4A \\sim O3A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Cl2 \\sim O3B \\sim O1B \\sim O4B \\sim O2B: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 Cl2, O1A, O2A, O3B, O4A, O1B, O3A, O4B, O2B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(O1B)=Sof(O3A)=Sof(O4B)=Sof(O2B)=1-FVAR(1)
 Sof(O1A)=Sof(O2A)=Sof(O3B)=Sof(O4A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C23(H23), C24(H24), C25(H25),
  C26(H26)
;
_shelx_res_checksum              14031
_shelx_fab_checksum              79366
_olex2_submission_special_instructions 'No special instructions were received'