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_7132660
_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         '3(H2 O), C10 H5 N2 O4, C5 H9 N2'
_chemical_formula_sum            'C15 H20 N4 O7'
_chemical_formula_weight         368.35
_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             2023-12-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec141 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-05 deposited with the CCDC.	2024-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.89(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.301(2)
_cell_length_b                   23.093(5)
_cell_length_c                   6.9978(14)
_cell_measurement_reflns_used    23203
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.874
_cell_volume                     1756.5(7)
_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
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0680
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            23203
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.992
_diffrn_reflns_theta_max         24.992
_diffrn_reflns_theta_min         1.874
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.547429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1423 before and 0.0670 after correction.
The Ratio of minimum to maximum transmission is 0.5474.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       needle
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         3082
_refine_ls_number_restraints     203
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0972
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1398P)^2^+4.9155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2889
_refine_ls_wR_factor_ref         0.3039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2463
_reflns_number_total             3082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06264c2.cif
_cod_data_source_block           nanny3
_cod_depositor_comments
'Adding full bibliography for 7132656--7132660.cif.'
_cod_original_cell_volume        1756.4(7)
_cod_database_code               7132660
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.980
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(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
 C9B-O3B
 2.3 with sigma of 0.02
 C9B-C10B
 1.5 with sigma of 0.02
 C8B-C10B
 2.5 with sigma of 0.02
 C5-C7B
 1.4 with sigma of 0.02
 C7B-C8B
 1.4 with sigma of 0.02
 C5-C8B
 2.4 with sigma of 0.02
 C10B-O4B
 1.25 with sigma of 0.02
 N2B-C9B
 1.35 with sigma of 0.02
 C9B-C8B
 1.4 with sigma of 0.02
 C7B-C9B
 2.4 with sigma of 0.02
 C5-N2B
 2.4 with sigma of 0.02
 N2B-C8B
 2.4 with sigma of 0.02
 N2B-C7B
 2.8 with sigma of 0.02
 C6-N2B
 1.35 with sigma of 0.02
 O3B-C10B
 1.35 with sigma of 0.02
3. Rigid bond restraints
 O3A, N2B, O4A, C10A, C7A, C8A, C9A, N2A, O3B, O4B, C10B, C9B, C8B, C7B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O6, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O3A \\sim N2B \\sim O4A \\sim C10A \\sim C7A \\sim C8A \\sim C9A \\sim N2A
\\sim O3B \\sim O4B \\sim C10B \\sim C9B \\sim C8B \\sim C7B: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
O6 \\sim O7: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(N2B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(O3A)=Sof(H3A)=Sof(O4A)=Sof(C10A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=
 Sof(C9A)=Sof(N2A)=1-FVAR(1)
 Sof(N2B)=Sof(O3B)=Sof(H3B)=Sof(O4B)=Sof(C10B)=Sof(C9B)=Sof(C8B)=Sof(H8B)=
 Sof(C7B)=Sof(H7B)=FVAR(1)
6.a Free rotating group:
 O5(H5A,H5B), O7(H7C,H7D), O6(H6A,H6B)
6.b Aromatic/amide H refined with riding coordinates:
 N3(H3C), N4(H4A), C3(H3), C4(H4), C7A(H7A), C8A(H8A), C13(H13), C8B(H8B),
 C7B(H7B)
6.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C)
6.d Idealised tetrahedral OH refined as rotating group:
 O3A(H3A), O3B(H3B)
;
_shelx_res_checksum              78233
_shelx_hkl_checksum              81709
_olex2_submission_special_instructions 'No special instructions were received'