Dinuclear copper(ii) complexes containing oxamate and blocking ligands: crystal structure, magnetic properties, and DFT calculations
Simões, Tatiana R. G.; do Pim, Walace D.; Metz, Karina C.; Ribeiro, Marcos A.; Valente, Daniel C. A.; Cardozo, Thiago M.; Pinheiro, Carlos B.; Pedroso, Emerson F.; Horta, Bruno A. C.; Pereira, Cynthia L. M.; de Souza, Gilmar P.; Stumpf, Humberto O.; New Journal of Chemistry 44 (2020) 2597–2608; doi:10.1039/C9NJ05584C

data_7059198
_publ_section_title
;
 Dinuclear copper(ii) complexes containing oxamate and blocking ligands:
 crystal structure, magnetic properties, and DFT calculations
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2597
_journal_page_last               2608
_journal_paper_doi               10.1039/C9NJ05584C
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C13 H16 Cu2 N4 O7, H2 O'
_chemical_formula_sum            'C13 H18 Cu2 N4 O8'
_chemical_formula_weight         485.39
_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             2019-09-20
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-07 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                76.242(5)
_cell_angle_beta                 88.366(6)
_cell_angle_gamma                73.715(6)
_cell_formula_units_Z            2
_cell_length_a                   6.9426(5)
_cell_length_b                   10.4944(7)
_cell_length_c                   11.9846(8)
_cell_measurement_reflns_used    2059
_cell_measurement_temperature    270.05(10)
_cell_measurement_theta_max      29.3595
_cell_measurement_theta_min      2.0757
_cell_volume                     813.42(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      270.05(10)
_diffrn_detector_area_resol_mean 10.4186
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -37.00   57.00   1.0000    3.5300
omega____ theta____ kappa____ phi______ frames
    -      -10.7980   77.0000 -150.0000 94

  2 omega   -9.00   92.00   1.0000    3.5300
omega____ theta____ kappa____ phi______ frames
    -       12.8293   77.0000  120.0000 101

  3 omega  -21.00   79.00   1.0000    3.5300
omega____ theta____ kappa____ phi______ frames
    -       12.8293   77.0000    0.0000 100
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0478911000
_diffrn_orient_matrix_UB_12      -0.0701067000
_diffrn_orient_matrix_UB_13      0.0036522000
_diffrn_orient_matrix_UB_21      0.0081041000
_diffrn_orient_matrix_UB_22      -0.0122674000
_diffrn_orient_matrix_UB_23      0.0606656000
_diffrn_orient_matrix_UB_31      -0.0946935000
_diffrn_orient_matrix_UB_32      -0.0134999000
_diffrn_orient_matrix_UB_33      0.0042134000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5904
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.082
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.670
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.389
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_description       block
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.5063
_exptl_crystal_size_mid          0.358
_exptl_crystal_size_min          0.0496
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3333
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0341P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2648
_reflns_number_total             3333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05584c2.cif
_cod_data_source_block           cudap_03
_cod_depositor_comments
;Adding full bibliography for 7059197--7059199.cif.

 Adding full bibliography for 7059197--7059199.cif.
;
_cod_database_code               7059198
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C13 H18 Cu2 N4 O8'
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.345
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups, All O(H,H,H,H) groups
2. Restrained distances
 OW1-HW1A = OW1-HW1B
 0.85 with sigma of 0.01
 OW2-HW2B = OW2-HW2A
 0.85 with sigma of 0.01
 HW1B-HW1A
 1.4 with sigma of 0.01
 HW2A-HW2B
 1.4 with sigma of 0.01
3.a Free rotating group:
 OW2(HW2A,HW2B,HW1A,HW1B)
3.b Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B), N3(H3A,H3B), C13(H13A,H13B), C11(H11A,H11B), C12(H12A,H12B)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9)
;
_shelx_res_checksum              46023
_olex2_submission_special_instructions 'No special instructions were received'