Structural and electrochemical properties of mononuclear copper(II) complexes with pentadentate ethylenediamine-based ligands with pyridine/quinoline/isoquinoline/quinoxaline binding sites.
Mikata, Yuji; Akedo, Miyu; Hamamoto, Erina; Yoshida, Shoko; Shoji, Sunao; Ohsedo, Yutaka; Matsuo, Takashi; Storr, Tim; Funahashi, Yasuhiro; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16716–16732; doi:10.1039/d4dt02363c

data_7717086
_publ_section_title
;
 Structural and electrochemical properties of mononuclear copper(II)
 complexes with pentadentate ethylenediamine-based ligands with
 pyridine/quinoline/isoquinoline/quinoxaline binding sites.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16716
_journal_page_last               16732
_journal_paper_doi               10.1039/d4dt02363c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C33 H31 Cu N5, 2(Cl O4), 0.5(C H Cl3), 0.5(C2 H3 N), C1 H4 O1'
_chemical_formula_sum            'C35.5 H37 Cl3.5 Cu N5.5 O9'
_chemical_formula_weight         872.32
_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   geom
_audit_creation_date             2024-08-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-08 deposited with the CCDC.	2024-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.021(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.6631(5)
_cell_length_b                   15.1459(3)
_cell_length_c                   28.2417(9)
_cell_measurement_reflns_used    17352
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.8860
_cell_measurement_theta_min      2.2480
_cell_volume                     7710.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.109a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.109a 64-bit (release 21-02-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.109a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.812
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -88.00  -7.00   0.50   30.00    --  -13.52 -46.00 -65.00  162
  2  \w    -40.00  64.00   0.50   30.00    --  -13.52  46.00  84.00  208
  3  \w     47.00  76.00   0.50   30.00    --   12.43 178.00 -60.00   58
  4  \w     46.00  88.00   0.50   30.00    --   12.43 178.00 -90.00   84
  5  \w    -99.00 -65.00   0.50   30.00    --  -13.52-178.00-180.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.812
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            55167
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.812
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.157
_diffrn_reflns_theta_min         2.009
_exptl_absorpt_coefficient_mu    0.870
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.109a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       plate
_exptl_crystal_F_000             3592
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.089
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         18533
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0706
_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^)+(0.1208P)^2^+11.5028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2010
_refine_ls_wR_factor_ref         0.2224
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12505
_reflns_number_total             18533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02363c2.cif
_cod_data_source_block           3-iso-metqen-cu(clo4)2-240614_autored
_cod_depositor_comments
'Adding full bibliography for 7717077--7717088.cif.'
_cod_original_formula_sum        'C35.50 H37 Cl3.50 Cu N5.50 O9'
_cod_database_code               7717086
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.859
_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) groups
2. Restrained distances
 C17-O67
 1.32 with sigma of 0.01
 O17-C68
 1.32 with sigma of 0.01
 C68A-O17A
 1.32 with sigma of 0.01
 C17A-O67A
 1.32 with sigma of 0.01
 O67-C17 \\sim O67A-C17A
 with sigma of 0.02
 O17-C68 \\sim O17A-C68A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O67A \\sim C17A \\sim O67 \\sim C17: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C68 \\sim C68A \\sim O17 \\sim O17A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(O17A) \\sim Ueq, Uanis(C68A) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(C68)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O67A, C17A, O67, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O17, C68, O17A, C68A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O67A)=Sof(H67B)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(O67)=Sof(H67A)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
 Sof(O17A)=Sof(H17G)=Sof(C68A)=Sof(H68D)=Sof(H68E)=Sof(H68F)=1-FVAR(2)
 Sof(O17)=Sof(H17)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C71(H71)
6.b Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C23(H23A,H23B), C2(H2A,H2B), C13(H13A,H13B), C35(H35A,H35B),
 C1(H1A,H1B), C36(H36A,H36B), C3(H3A,H3B), C34(H34A,H34B), C46(H46A,H46B)
6.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C26(H26), C57(H57), C14(H14), C30(H30), C4(H4), C6(H6), C28(H28),
 C16(H16), C59(H59), C47(H47), C29(H29), C10(H10), C7(H7), C37(H37), C67(H67),
 C27(H27), C20(H20), C43(H43), C39(H39), C63(H63), C62(H62), C8(H8), C53(H53),
 C18(H18), C9(H9), C60(H60), C19(H19), C61(H61), C49(H49), C40(H40), C42(H42),
 C41(H41), C52(H52), C50(H50), C51(H51)
6.d Tetrahedral OH refined with riding coordinates:
 O67A(H67B), O17(H17), O17A(H17G)
6.e Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C66(H66A,H66B,H66C), C70(H70A,H70B,H70C), C17(H17A,H17B,
 H17C), C17A(H17D,H17E,H17F), C68(H68A,H68B,H68C), C68A(H68D,H68E,H68F)
6.f Idealised tetrahedral OH refined as rotating group:
 O67(H67A)
;
_shelx_res_checksum              21870
_shelx_hkl_checksum              51416
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;