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_7132657
_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         'C12 H20 Cu F6 N4 O8 S2'
_chemical_formula_sum            'C12 H20 Cu F6 N4 O8 S2'
_chemical_formula_weight         589.98
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2023-12-04
_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                 110.87(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.686(2)
_cell_length_b                   14.011(3)
_cell_length_c                   8.0619(16)
_cell_measurement_reflns_used    16643
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      2.908
_cell_volume                     1127.8(5)
_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)'
_computing_structure_solution    'ShelXT-2016 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k-geometry 4 circles diffractometer'
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaAPEXII'
_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  0.0359
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16643
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.908
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.249
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.728060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1738 before and 0.0401 after correction.
The Ratio of minimum to maximum transmission is 0.7281.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       plate
_exptl_crystal_F_000             598
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2574
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0457P)^2^+0.5346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0841
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2347
_reflns_number_total             2574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06264c2.cif
_cod_data_source_block           sad2
_cod_depositor_comments
'Adding full bibliography for 7132656--7132660.cif.'
_cod_original_cell_volume        1127.8(4)
_cod_database_code               7132657
_shelx_shelxl_version_number     2019/3
_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 C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 F3B-C6
 1.32 with sigma of 0.02
 C6-F1B
 1.32 with sigma of 0.02
 C6-F2B
 1.32 with sigma of 0.02
 F3B-F1B
 2.1 with sigma of 0.02
 F3B-F2B
 2.1 with sigma of 0.02
 F1B-F2B
 2.1 with sigma of 0.02
 F2B-F2A
 0.9 with sigma of 0.02
 O2B-S1
 1.4 with sigma of 0.02
 S1-O3B
 1.4 with sigma of 0.02
 S1-O4B
 1.4 with sigma of 0.02
3. Rigid bond restraints
 F2A, F1A, F3A, C6, F3B, F1B, F2B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S1, O2A, O4A, O3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S1, O2A, O4A, O3A, O2B, O4B, O3B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F2A \\sim F1A \\sim F3A \\sim C6 \\sim F3B \\sim F1B \\sim F2B: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
S1 \\sim O2A \\sim O4A \\sim O3A: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
S1 \\sim O2A \\sim O4A \\sim O3A \\sim O2B \\sim O4B \\sim O3B: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
Uanis(F1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F3B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F2B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(F3B)=Sof(F1B)=Sof(F2B)=1-FVAR(1)
 Sof(F2A)=Sof(F1A)=Sof(F3A)=FVAR(1)
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=1-FVAR(2)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=FVAR(2)
 Sof(O2B)=Sof(O4B)=Sof(O3B)=1-FVAR(3)
 Sof(O2A)=Sof(O4A)=Sof(O3A)=FVAR(3)
6.a Rotating group:
 O1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3)
6.c Idealised Me refined as rotating group:
 C1(H1AA,H1AB,H1AC), C1(H1BD,H1BE,H1BF), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              56805
_shelx_hkl_checksum              59847
_olex2_submission_special_instructions 'No special instructions were received'