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_7717088
_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         'C39 H35 Cu N5, 2(Cl O4), 1.25(C2 H3 N)'
_chemical_formula_sum            'C41.5 H38.75 Cl2 Cu N6.25 O8'
_chemical_formula_weight         887.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                76.205(10)
_cell_angle_beta                 86.332(9)
_cell_angle_gamma                87.694(8)
_cell_formula_units_Z            4
_cell_length_a                   13.425(6)
_cell_length_b                   15.738(7)
_cell_length_c                   19.413(8)
_cell_measurement_reflns_used    8210
_cell_measurement_temperature    153
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.60
_cell_volume                     3974(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_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    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      153.15
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40334
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.421
_exptl_absorpt_coefficient_mu    0.747
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1834
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.296
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1187
_refine_ls_number_reflns         17833
_refine_ls_number_restraints     565
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0635
_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^)+(0.1170P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1621
_refine_ls_wR_factor_ref         0.2045
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11046
_reflns_number_total             17833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02363c2.cif
_cod_data_source_block           3isobntqen-cu(clo4)2-210604
_cod_depositor_comments
'Adding full bibliography for 7717077--7717088.cif.'
_cod_original_formula_sum        'C41.50 H38.75 Cl2 Cu N6.25 O8'
_cod_database_code               7717088
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.865
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H80A,H80B,H80C} of C80, All C(H,H) groups
 At 1.5 times of:
  {H1CA,H1CB,H1CC} of C1C, {H1EA,H1EB,H1EC} of C1E, {H1BA,H1BB,H1BC} of C1B
2. Restrained distances
 Cl4-O13 = Cl4-O14 = Cl4-O15 = Cl4-O16
 1.5 with sigma of 0.02
 N12-C1A
 1.14 with sigma of 0.02
 C1A-N12
 1.137 with sigma of 0.01
 C1A-C1B
 1.456 with sigma of 0.01
 C1B-N12
 2.593 with sigma of 0.02
 Cl3-O9 = Cl3-O10 = Cl3-O11 = Cl3-O12
 1.5 with sigma of 0.02
 N13-C1D
 1.14 with sigma of 0.02
 C1D-N13
 1.137 with sigma of 0.01
 C1D-C1E
 1.456 with sigma of 0.01
 C1E-N13
 2.593 with sigma of 0.02
 N12-C1B
 2.59 with sigma of 0.04
 N13-C1E
 2.59 with sigma of 0.04
 Cl4-O13 \\sim Cl4-O14 \\sim Cl4-O15 \\sim Cl4-O16
 with sigma of 0.02
 O13-O15 \\sim O14-O16 \\sim O13-O16 \\sim O14-O15 \\sim O13-O14 \\sim O15-O16
 with sigma of 0.04
 Cl4-O13 \\sim Cl4-O13A
 with sigma of 0.02
 Cl4-O14 \\sim Cl4-O14A
 with sigma of 0.02
 N12-C1A \\sim N12A-C81
 with sigma of 0.02
 Cl4-O15 \\sim Cl4-O15A
 with sigma of 0.02
 Cl4-O16 \\sim Cl4-O16A
 with sigma of 0.02
 C1A-C1B \\sim C81-C1C
 with sigma of 0.02
 N12-C1B \\sim N12A-C1C
 with sigma of 0.04
 Cl3-O9 \\sim Cl3-O10 \\sim Cl3-O11 \\sim Cl3-O12
 with sigma of 0.02
 O9-O11 \\sim O10-O12 \\sim O9-O12 \\sim O10-O11 \\sim O9-O10 \\sim O11-O12
 with sigma of 0.04
 Cl3-O9 \\sim Cl3A-O9A
 with sigma of 0.02
 Cl3-O10 \\sim Cl3A-O10A
 with sigma of 0.02
 Cl3-O11 \\sim Cl3A-O11A
 with sigma of 0.02
 Cl3-O12 \\sim Cl3A-O12A
 with sigma of 0.02
 O9-O10 \\sim O9A-O10A
 with sigma of 0.04
 O9-O11 \\sim O9A-O11A
 with sigma of 0.04
 O9-O12 \\sim O9A-O12A
 with sigma of 0.04
 O10-O11 \\sim O10A-O11A
 with sigma of 0.04
 O10-O12 \\sim O10A-O12A
 with sigma of 0.04
 O11-O12 \\sim O11A-O12A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cl4 \\sim O13 \\sim O14 \\sim O15 \\sim O16: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
N12 \\sim C1A \\sim C1B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O13 \\sim Cl4 \\sim O16 \\sim O13A \\sim O14A \\sim O15A \\sim O14 \\sim O15
\\sim O16A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C1A \\sim N12 \\sim C1B \\sim N12A \\sim C81 \\sim C1C: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Cl3 \\sim O9 \\sim O10 \\sim O11 \\sim O12: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Cl3 \\sim O9 \\sim O11 \\sim O10 \\sim O12 \\sim Cl3A \\sim O9A \\sim O11A
\\sim O10A \\sim O12A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
N13 \\sim C1D \\sim C1E: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 Cl4, O13, O14, O15, O16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N12, C1A, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O13, Cl4, O16, O13A, O14A, O15A, O14, O15, O16A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, N12, C1A, N12A, C81, C1C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl3, O9, O10, O11, O12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O12, Cl3, O9, O11, O10, O12A, O9A, Cl3A, O11A, O10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N13, C1D, C1E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O15A)=Sof(O16A)=Sof(O14A)=Sof(O13A)=1-FVAR(1)
 Sof(O13)=Sof(O14)=Sof(O15)=Sof(O16)=FVAR(1)
 Sof(O9A)=Sof(O11A)=Sof(Cl3A)=Sof(O10A)=Sof(O12A)=1-FVAR(2)
 Sof(Cl3)=Sof(O9)=Sof(O10)=Sof(O11)=Sof(O12)=FVAR(2)
 Sof(N12A)=Sof(C81)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=1-FVAR(3)
 Sof(N12)=Sof(C1A)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=FVAR(3)
 Fixed Sof: N13(0.5) C1D(0.5) C1E(0.5) H1EA(0.5) H1EB(0.5) H1EC(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C13(H13A,H13B), C23(H23A,H23B),
 C33(H33A,H33B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C52(H52A,H52B),
  C62(H62A,H62B), C72(H72A,H72B)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C24(H24), C26(H26), C27(H27), C28(H28),
  C29(H29), C30(H30), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39),
 C43(H43), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C53(H53), C55(H55),
  C56(H56), C57(H57), C58(H58), C59(H59), C63(H63), C65(H65), C66(H66),
 C67(H67), C68(H68), C69(H69), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78)
6.c Idealised Me refined as rotating group:
 C80(H80A,H80B,H80C), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1E(H1EA,H1EB,
 H1EC)
;
_shelx_res_checksum              20582
_shelx_hkl_checksum              52280
_olex2_submission_special_instructions 'No special instructions were received'