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_7717080
_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         'C34 H31 Cu N5, 2(Cl O4), 0.5(C2 H3 N)'
_chemical_formula_sum            'C35 H32.5 Cl2 Cu N5.5 O8'
_chemical_formula_weight         792.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-06-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-06 deposited with the CCDC.	2024-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.504(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.9174(2)
_cell_length_b                   18.9067(4)
_cell_length_c                   37.0398(7)
_cell_measurement_reflns_used    13111
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      29.2090
_cell_measurement_theta_min      2.3040
_cell_volume                     6942.8(2)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.864
_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     46.00  78.00   0.50   25.00    --   17.93-138.00 164.00   64
  2  \w    -78.00 -53.00   0.50   25.00    --  -19.03 132.00  50.00   50
  3  \w    -94.00 -43.00   0.50   25.00    --  -19.03 138.00-133.00  102
  4  \w     45.00  99.00   0.50   25.00    --   17.93 178.00 -30.00  108
  5  \w     44.00 100.00   0.50   25.00    --   17.93 178.00-120.00  112
  6  \w    -25.00  63.00   0.50   25.00    --  -19.03  19.00 -90.00  176
  7  \w    -26.00  56.00   0.50   25.00    --  -19.03  19.00-180.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0026064000
_diffrn_orient_matrix_UB_12      -0.0361935000
_diffrn_orient_matrix_UB_13      0.0050165000
_diffrn_orient_matrix_UB_21      0.0138466000
_diffrn_orient_matrix_UB_22      -0.0099444000
_diffrn_orient_matrix_UB_23      -0.0179811000
_diffrn_orient_matrix_UB_31      0.0701383000
_diffrn_orient_matrix_UB_32      0.0006034000
_diffrn_orient_matrix_UB_33      0.0042500000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            26753
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.498
_diffrn_reflns_theta_min         2.154
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91250
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       plate
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.396
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         8373
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0726P)^2^+11.8214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1402
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6814
_reflns_number_total             8373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02363c2.cif
_cod_data_source_block           ph-pqq-cu(clo4)2-240523_autored
_cod_depositor_comments
'Adding full bibliography for 7717077--7717088.cif.'
_cod_original_formula_sum        'C35 H32.50 Cl2 Cu N5.50 O8'
_cod_database_code               7717080
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C34H31N5CuCl2O8
_chemical_oxdiff_usercomment     akedo
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.863
_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
2. Restrained distances
 Cl2-O8 \\sim Cl2-O9
 with sigma of 0.02
 Cl2-O10 \\sim Cl2-O11
 with sigma of 0.02
 O10-O9 \\sim O11-O9
 with sigma of 0.02
 Cl2-O6 \\sim Cl2-O7
 with sigma of 0.02
 O6-O11 \\sim O7-O11
 with sigma of 0.02
3. Others
 Sof(O9)=1-FVAR(1)
 Sof(O8)=FVAR(1)
 Sof(O11)=1-FVAR(2)
 Sof(O10)=FVAR(2)
 Sof(O7)=1-FVAR(3)
 Sof(O6)=FVAR(3)
 Fixed Sof: H36A(0.5) H36B(0.5) H36C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C9(H9A,H9B), C3(H3A,H3B), C1(H1A,H1B), C2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C26(H26), C22(H22), C25(H25), C16(H16), C15(H15), C34(H34),
 C24(H24), C30(H30), C12(H12), C33(H33), C23(H23), C8(H8), C11(H11), C31(H31),
 C32(H32), C7(H7), C13(H13), C14(H14), C5(H5), C6(H6)
4.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              20813
_shelx_hkl_checksum              89550
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.113
_oxdiff_exptl_absorpt_empirical_full_min 0.855