Synthesis of unsymmetrical 1,8-naphthyridine-based ligands for the assembly of tri-and tetra-nuclear copper(ii) complexes
Bacher, Felix; Isaac, James A.; Philouze, Christian; Flot, David; Thibon-Pourret, Aurore; Belle, Catherine; New Journal of Chemistry 44 (2020) 16713–16720; doi:10.1039/D0NJ02776F

data_7059824
_publ_section_title
;
 Synthesis of unsymmetrical 1,8-naphthyridine-based ligands for the
 assembly of tri-and tetra-nuclear copper(ii) complexes
;
_journal_issue                   39
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16713
_journal_page_last               16720
_journal_paper_doi               10.1039/D0NJ02776F
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety
'C54 H40 Cu4 N10 O6, 2(C F3 O3 S), 2(C3 H7 N O)'
_chemical_formula_sum            'C62 H54 Cu4 F6 N12 O14 S2'
_chemical_formula_weight         1623.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2019-12-10 deposited with the CCDC.	2020-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.06(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.475(5)
_cell_length_b                   12.394(3)
_cell_length_c                   22.723(5)
_cell_measurement_reflns_used    27897
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.998
_cell_measurement_theta_min      2.584
_cell_volume                     6329(3)
_computing_cell_refinement       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '\k-geometry 4 circles diffractometer'
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaAPEXII'
_diffrn_measurement_method       'Phi and omega 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  0.0793
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27897
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.584
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.487
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.245699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.6065 before and 0.0898 after correction.
The Ratio of minimum to maximum transmission is 0.2457.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_description       plate
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.119
_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     505
_refine_ls_number_reflns         6189
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0550P)^2^+44.5733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4960
_reflns_number_total             6189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02776f2.cif
_cod_data_source_block           sad
_cod_depositor_comments
'Adding full bibliography for 7059823--7059825.cif.'
_cod_original_cell_volume        6329(2)
_cod_database_code               7059824
_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. Rigid bond restraints
 N6A, O7A, C29A, C30A, C31A, N6B, O7B, C29B, C31B, C30B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C30A \\sim O7A \\sim C29A \\sim N6A \\sim C31A \\sim N6B \\sim O7B \\sim C29B
\\sim C31B \\sim C30B: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Others
 Sof(O7B)=Sof(N6B)=Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C29B)=Sof(H29B)=
 Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(O7A)=Sof(N6A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=
 Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
5.a Free rotating group:
 O3(H3)
5.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C2(H2), C3(H3A), C11(H11), C17(H17), C6(H6), C26(H26), C24(H24),
 C25(H25), C19(H19), C23(H23), C18(H18), C16(H16), C13(H13), C7(H7), C12(H12),
 C29A(H29A), C29B(H29B)
5.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C31B(H31D,H31E,H31F), C30B(H30D,H30E,H30F), C30A(H30A,
 H30B,H30C), C31A(H31A,H31B,H31C)
;
_shelx_res_checksum              85595
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'