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_7047825
_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         'C44 H46 Cu2 N8 O2, 4(Cl1 O4)'
_chemical_formula_sum            'C44 H46 Cl4 Cu2 N8 O18'
_chemical_formula_weight         1243.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-13
_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                109.7640(10)
_cell_angle_beta                 95.8450(10)
_cell_angle_gamma                97.6530(10)
_cell_formula_units_Z            1
_cell_length_a                   10.0380(3)
_cell_length_b                   10.6269(3)
_cell_length_c                   12.7725(4)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.816
_cell_measurement_theta_min      2.929
_cell_volume                     1254.94(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 D8 QUEST CMOS'
_diffrn_measurement_method       '\w and \f 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  0.0401
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            42084
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.921
_diffrn_reflns_theta_min         2.929
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I\mus'
_exptl_absorpt_coefficient_mu    1.143
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0602 before and 0.0499 after correction.
The Ratio of minimum to maximum transmission is 0.9162.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         5996
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0590P)^2^+1.0051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1175
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4727
_reflns_number_total             5996
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03183e2.cif
_cod_data_source_block           pl7
_cod_depositor_comments
'Adding full bibliography for 7047824--7047826.cif.'
_cod_database_code               7047825
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.755
_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. Restrained distances
 O6A-O8A \\sim O6A-O7A \\sim O6A-O9A \\sim O8A-O7A \\sim O8A-O9A \\sim O7A-O9A
 with sigma of 0.04
 Cl2A-O6A \\sim Cl2A-O8A \\sim Cl2A-O7A \\sim Cl2A-O9A
 with sigma of 0.02
 O6B-O8B \\sim O6B-O7B \\sim O6B-O9B \\sim O8B-O7B \\sim O8B-O9B \\sim O7B-O9B
 with sigma of 0.04
 Cl2B-O6B \\sim Cl2B-O8B \\sim Cl2B-O7B \\sim Cl2B-O9B
 with sigma of 0.02
 O4A-O2A \\sim O4A-O5A \\sim O2A-O5A \\sim O2B-O4B \\sim O2B-O5B \\sim O4B-O5B
 with sigma of 0.04
 Cl1-O3 \\sim Cl1-O4A \\sim Cl1-O2A \\sim Cl1-O5A \\sim Cl1-O2B \\sim Cl1-O4B
\\sim Cl1-O5B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Cl1, O3, O4A, O2A, O5A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl2A, O6A, O8A, O7A, O9A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl1, O3, O2B, O4B, O5B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl2B, O6B, O8B, O7B, O9B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(Cl2B)=Sof(O6B)=Sof(O8B)=Sof(O7B)=Sof(O9B)=1-FVAR(1)
 Sof(Cl2A)=Sof(O6A)=Sof(O8A)=Sof(O7A)=Sof(O9A)=FVAR(1)
 Sof(O2B)=Sof(O4B)=Sof(O5B)=1-FVAR(2)
 Sof(O4A)=Sof(O2A)=Sof(O5A)=FVAR(2)
5.a Rotating group:
 O1(H1A,H1B)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B)
5.c 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)
5.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_shelx_res_checksum              81168
_olex2_submission_special_instructions 'No special instructions were received'