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_7717085
_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
'C30 H29 Cu N5, 2(Cl O4), 0.75(C H4 O), 0.125(H2 O)'
_chemical_formula_sum            'C30.75 H32.25 Cl2 Cu N5 O8.88'
_chemical_formula_weight         748.30
_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
_audit_creation_date             2024-08-07
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-07 deposited with the CCDC.	2024-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.788(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   8.1238(2)
_cell_length_b                   37.8829(8)
_cell_length_c                   41.6362(12)
_cell_measurement_reflns_used    16086
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      29.3750
_cell_measurement_theta_min      2.1440
_cell_volume                     12798.5(6)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     28.00  53.46   0.38   30.00    --   17.78-132.00-141.00   67
  2  \w     56.00  81.08   0.38   30.00    --   17.78-137.00  42.00   66
  3  \w    -93.00 -22.70   0.38   30.00    --  -18.87 137.00 104.00  185
  4  \w    -54.00 -27.78   0.38   30.00    --  -18.87 132.00 -71.00   69
  5  \w    -61.00 -33.64   0.38   30.00    --   17.78 -19.00 150.00   72
  6  \w     42.00  99.00   0.38   30.00    --   17.78-178.00  30.00  150
  7  \w    -26.00  13.14   0.38   30.00    --  -18.87  19.00 -30.00  103
  8  \w     23.00  49.22   0.38   30.00    --  -18.87  19.00 -30.00   69
  9  \w    -26.00  61.02   0.38   30.00    --  -18.87  19.00-120.00  229
;
_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  0.0635
_diffrn_reflns_av_unetI/netI     0.0843
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            83201
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.150
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.109a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       needle
_exptl_crystal_F_000             6172
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1879
_refine_ls_number_reflns         23294
_refine_ls_number_restraints     687
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1167
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0654P)^2^+6.9313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13744
_reflns_number_total             23294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02363c2.cif
_cod_data_source_block           ph-pq_autored
_cod_depositor_comments
'Adding full bibliography for 7717077--7717088.cif.'
_cod_database_code               7717085
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.860
_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, All O(H,H) groups
2. Restrained distances
 Cl2-O5 = Cl2-O6 = Cl2-O7 = Cl2-O8
 1.5 with sigma of 0.02
 O17-C1A
 1.33 with sigma of 0.01
 Cl3-O10 = Cl3-O11 = Cl3-O12 = Cl3-O13
 1.5 with sigma of 0.02
 H1BC-C78
 2.52 with sigma of 0.01
 H1AC-C77
 3.2 with sigma of 0.01
 Cl4-O9 = Cl4-O14 = Cl4-O15 = Cl4-O16
 1.5 with sigma of 0.02
 H62A-H1CA
 2.2 with sigma of 0.01
 O17-C1A \\sim O17A-C1B
 with sigma of 0.01
 Cl3-O10 \\sim Cl3-O11 \\sim Cl3-O12 \\sim Cl3-O13
 with sigma of 0.02
 Cl4-O9 \\sim Cl4-O14 \\sim Cl4-O15 \\sim Cl4-O16
 with sigma of 0.02
 O10-O12 \\sim O11-O13 \\sim O10-O13 \\sim O11-O12 \\sim O10-O11 \\sim O12-O13
 with sigma of 0.04
 Cl2-O5 \\sim Cl2-O6 \\sim Cl2-O7 \\sim Cl2-O8
 with sigma of 0.02
 Cl3-O10 \\sim Cl3-O10A
 with sigma of 0.02
 O5-O7 \\sim O6-O8 \\sim O5-O8 \\sim O6-O7 \\sim O5-O6 \\sim O7-O8
 with sigma of 0.04
 Cl3-O11 \\sim Cl3-O11A
 with sigma of 0.02
 O9-O15 \\sim O14-O16 \\sim O9-O16 \\sim O14-O15 \\sim O9-O14 \\sim O15-O16
 with sigma of 0.04
 Cl3-O12 \\sim Cl3-O12A
 with sigma of 0.02
 Cl3-O13 \\sim Cl3-O13A
 with sigma of 0.02
 Cl4-O9 \\sim Cl4A-O9A
 with sigma of 0.02
 Cl4-O14 \\sim Cl4A-O14A
 with sigma of 0.02
 Cl2-O5 \\sim Cl2A-O5A
 with sigma of 0.02
 Cl4-O15 \\sim Cl4A-O15A
 with sigma of 0.02
 Cl4-O16 \\sim Cl4A-O16A
 with sigma of 0.02
 Cl2-O6 \\sim Cl2A-O6A
 with sigma of 0.02
 Cl2-O7 \\sim Cl2A-O7A
 with sigma of 0.02
 O9-O14 \\sim O9A-O14A
 with sigma of 0.04
 O9-O15 \\sim O9A-O15A
 with sigma of 0.04
 Cl2-O8 \\sim Cl2A-O8A
 with sigma of 0.02
 O9-O16 \\sim O9A-O16A
 with sigma of 0.04
 O5-O6 \\sim O5A-O6A
 with sigma of 0.04
 O5-O7 \\sim O5A-O7A
 with sigma of 0.04
 O14-O15 \\sim O14A-O15A
 with sigma of 0.04
 O14-O16 \\sim O14A-O16A
 with sigma of 0.04
 O5-O8 \\sim O5A-O8A
 with sigma of 0.04
 O6-O7 \\sim O6A-O7A
 with sigma of 0.04
 O15-O16 \\sim O15A-O16A
 with sigma of 0.04
 O6-O8 \\sim O6A-O8A
 with sigma of 0.04
 O7-O8 \\sim O7A-O8A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C1A \\sim O17 \\sim C1B \\sim O17A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Cl2 \\sim O5 \\sim O6 \\sim O7 \\sim O8: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
O11A \\sim Cl3 \\sim O12 \\sim O11 \\sim O12A \\sim O10 \\sim O10A \\sim O13A
\\sim O13: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O16 \\sim Cl4 \\sim O9 \\sim O14 \\sim O15 \\sim O16A \\sim Cl4A \\sim O9A
\\sim O14A \\sim O15A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C1C \\sim O1A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(O17A) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(O17)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O36) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C1A, O17, C1B, O17A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2, O5, O6, O7, O8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O11A, Cl3, O12, O11, O12A, O10, O10A, O13A, O13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O15A, O16A, Cl4A, O9A, O14A, O16, Cl4, O9, O14, O15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1A, C1C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(O6A)=Sof(Cl2A)=Sof(O7A)=Sof(O5A)=Sof(O8A)=1-FVAR(1)
 Sof(Cl2)=Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=FVAR(1)
 Sof(O16A)=Sof(Cl4A)=Sof(O9A)=Sof(O14A)=Sof(O15A)=1-FVAR(2)
 Sof(Cl4)=Sof(O9)=Sof(O14)=Sof(O15)=Sof(O16)=FVAR(2)
 Sof(O11A)=Sof(O10A)=Sof(O12A)=Sof(O13A)=1-FVAR(3)
 Sof(O10)=Sof(O11)=Sof(O12)=Sof(O13)=FVAR(3)
 Sof(O17A)=Sof(H17B)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=1-FVAR(4)
 Sof(O17)=Sof(H17A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=FVAR(4)
 Fixed Sof: O36(0.5) H36A(0.5) H36B(0.5)
6.a Free rotating group:
 O36(H36A,H36B), O17(C1A), O17A(C1B), O1A(C1C)
6.b Secondary CH2 refined with riding coordinates:
 C93(H93A,H93B), C2(H2A,H2B), C9(H9A,H9B), C15(H15A,H15B), C105(H10A,H10B),
 C99(H99A,H99B), C45(H45A,H45B), C92(H92A,H92B), C1(H1A,H1B), C91(H91A,H91B),
 C3(H3A,H3B), C32(H32A,H32B), C31(H31A,H31B), C75(H75A,H75B), C69(H69A,H69B),
 C62(H62A,H62B), C61(H61A,H61B), C39(H39A,H39B), C33(H33A,H33B), C63(H63A,H63B)
6.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C8(H8), C52(H52), C13(H13), C104(H104), C101(H101), C98(H98),
 C51(H51), C102(H102), C5(H5), C60(H60), C21(H21), C22(H22), C44(H44), C12(H12),
  C96(H96), C17(H17), C18(H18), C30(H30), C112(H112), C20(H20), C48(H48),
 C49(H49), C26(H26), C50(H50), C111(H111), C28(H28), C97(H97), C56(H56),
 C103(H103), C95(H95), C11(H11), C47(H47), C29(H29), C7(H7), C27(H27), C19(H19),
  C6(H6), C116(H116), C110(H110), C74(H74), C59(H59), C109(H109), C120(H120),
 C82(H82), C43(H43), C68(H68), C71(H71), C107(H107), C38(H38), C57(H57),
 C58(H58), C77(H77), C72(H72), C79(H79), C67(H67), C119(H119), C80(H80),
 C42(H42), C108(H108), C73(H73), C78(H78), C117(H117), C66(H66), C81(H81),
 C41(H41), C86(H86), C118(H118), C65(H65), C90(H90), C37(H37), C88(H88),
 C87(H87), C89(H89), C122(H122), C36(H36)
6.d Idealised Me refined as rotating group:
 C121(H12A,H12B,H12C), C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,
 H1CC)
6.e Idealised tetrahedral OH refined as rotating group:
 O34(H34), O17(H17A), O17A(H17B), O1A(H1AD)
;
_shelx_res_checksum              66150
_shelx_hkl_checksum              86814
_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
;