Insights into non-covalent interactions in dicopper(II,II) complexes bearing a naphthyridine scaffold: anion-dictated electrochemistry.
De Tovar, Jonathan; Philouze, Christian; Thibon-Pourret, Aurore; Belle, Catherine; Chemical communications (Cambridge, England) 60 (2024) 2228–2231; doi:10.1039/d3cc06264c

data_7132656
_publ_section_title
;
 Insights into non-covalent interactions in dicopper(II,II) complexes
 bearing a naphthyridine scaffold: anion-dictated electrochemistry.
;
_journal_issue                   16
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2228
_journal_page_last               2231
_journal_paper_doi               10.1039/d3cc06264c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C30 H36 Cu2 N10 O2, 2(Cl O4), 2(C3 H6 O)'
_chemical_formula_sum            'C36 H48 Cl2 Cu2 N10 O12'
_chemical_formula_weight         1010.82
_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   mixed
_audit_creation_date             2024-01-16
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec141 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-16 deposited with the CCDC.	2024-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                106.82(3)
_cell_angle_beta                 96.99(3)
_cell_angle_gamma                110.12(3)
_cell_formula_units_Z            2
_cell_length_a                   11.652(2)
_cell_length_b                   13.232(3)
_cell_length_c                   16.020(3)
_cell_measurement_reflns_used    51188
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      1.370
_cell_volume                     2151.7(11)
_computing_cell_refinement       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_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)'
_diffrn_ambient_temperature      200.00
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '\k-geometry 4 circles diffractometer'
_diffrn_measurement_device_type  Incoatec-Bruker-AXS-enraf-noniusKappaAPEXII
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51188
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.370
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.185
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.741443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.0731 before and 0.0304 after correction.
The Ratio of minimum to maximum transmission is 0.7414.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       plate
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         9831
_refine_ls_number_restraints     311
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0310P)^2^+1.7934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0804
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8665
_reflns_number_total             9831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06264c2.cif
_cod_data_source_block           recup
_cod_depositor_comments
'Adding full bibliography for 7132656--7132660.cif.'
_cod_original_cell_volume        2151.7(9)
_cod_database_code               7132656
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O12A-C34A
 1.2 with sigma of 0.02
 C34A-C35A
 1.5 with sigma of 0.02
 C34A-C33A
 1.5 with sigma of 0.02
 O12A-C35A
 2.3 with sigma of 0.02
 O12A-C33A
 2.3 with sigma of 0.02
 C35A-C33A
 2.5 with sigma of 0.02
 O12B-C34B
 1.2 with sigma of 0.02
 C35B-C34B
 1.5 with sigma of 0.02
 C34B-C33B
 1.5 with sigma of 0.02
 O12B-C35B
 2.3 with sigma of 0.02
 O12B-C33B
 2.3 with sigma of 0.02
 C35B-C33B
 2.5 with sigma of 0.02
3. Rigid bond restraints
 Cl2, O8A, O10A, O9A, O8B, O7B, O7A, O10B, O9B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C34B, C33B, O12B, C35B, O12A, C34A, C35A, C33A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O12A, C35B, C34A, C34B, O12B, C33A, C33B, C35A, O12C, C33C, C34C, C35C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl2 \\sim O8A \\sim O10A \\sim O9A \\sim O8B \\sim O7B \\sim O7A \\sim O10B
\\sim O9B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 1.7A
O12B \\sim C33B \\sim C34B \\sim C35B \\sim C33A \\sim O12A \\sim C34A \\sim
C35A \\sim O12C \\sim C33C \\sim C34C \\sim C35C: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 1.7A
O12A \\sim O12B \\sim C34B \\sim C34A \\sim C35B \\sim C33A \\sim C33B \\sim
C35A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 1.7A
5. Others
 Sof(O8A)=Sof(O10A)=Sof(O9A)=Sof(O7A)=1-FVAR(1)
 Sof(O8B)=Sof(O7B)=Sof(O10B)=Sof(O9B)=FVAR(1)
 Sof(C33B)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(O12B)=Sof(C34B)=Sof(C35B)=
 Sof(H35D)=Sof(H35E)=Sof(H35F)=0.8*(1-FVAR(3))
 Sof(O12A)=Sof(C34A)=Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C33A)=
 Sof(H33A)=Sof(H33B)=Sof(H33C)=0.8*FVAR(3)
 Fixed Sof: O12C(0.2) C34C(0.2) C33C(0.2) H33G(0.2) H33H(0.2) H33I(0.2)
 C35C(0.2) H35G(0.2) H35H(0.2) H35I(0.2)
6.a Free rotating group:
 O1(H1), O2(H2)
6.b Ternary CH refined with riding coordinates:
 C00T(H00T), C9(H9)
6.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C17(H17), C22(H22), C12(H12), C7(H7), C2(H2A), C6(H6), C3(H3)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C29(H29A,H29B,H29C), C20(H20A,H20B,
 H20C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C19(H19A,H19B,H19C), C25(H25A,
 H25B,H25C), C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C35A(H35A,H35B,H35C),
 C33A(H33A,H33B,H33C), C33B(H33D,H33E,H33F), C35B(H35D,H35E,H35F), C33C(H33G,
 H33H,H33I), C35C(H35G,H35H,H35I)
;
_shelx_res_checksum              85886
_shelx_hkl_checksum              58795
_olex2_submission_special_instructions 'No special instructions were received'