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_7059199
_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         'C12 H14 Cu2 N4 O7, 4(H2 O)'
_chemical_formula_sum            'C12 H22 Cu2 N4 O11'
_chemical_formula_weight         525.41
_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             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                90
_cell_angle_beta                 92.1980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.67460(10)
_cell_length_b                   17.3302(2)
_cell_length_c                   16.4950(2)
_cell_measurement_reflns_used    31878
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      29.4160
_cell_measurement_theta_min      3.0450
_cell_volume                     1906.61(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4186
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -67.00    3.00   1.0000   27.5700
omega____ theta____ kappa____ phi______ frames
    -      -10.7717  123.0000  139.0000 70

  2 omega  -57.00   17.00   1.0000   27.5700
omega____ theta____ kappa____ phi______ frames
    -      -10.7717  107.0000 -146.0000 74

  3 omega  -88.00  -26.00   1.0000   27.5700
omega____ theta____ kappa____ phi______ frames
    -      -10.7717  154.0000    6.0000 62

  4 omega  -21.00   85.00   1.0000   27.5700
omega____ theta____ kappa____ phi______ frames
    -       12.8029   77.0000   90.0000 106

  5 omega   -2.00   89.00   1.0000   27.5700
omega____ theta____ kappa____ phi______ frames
    -       12.8029   38.0000   30.0000 91

  6 omega  -14.00   89.00   1.0000   27.5700
omega____ theta____ kappa____ phi______ frames
    -       12.8029   38.0000  -60.0000 103

  7 omega  -66.00   46.00   1.0000   27.5700
omega____ theta____ kappa____ phi______ frames
    -       12.8029  -77.0000    0.0000 112

  8 omega  -87.00   16.00   1.0000   27.5700
omega____ theta____ kappa____ phi______ frames
    -      -10.7717  -38.0000 -150.0000 103

  9 omega  -44.00   68.00   1.0000   27.5700
omega____ theta____ kappa____ phi______ frames
    -      -10.7717   77.0000  -30.0000 112

 10 omega  -34.00   18.00   1.0000   27.5700
omega____ theta____ kappa____ phi______ frames
    -       12.8029  107.0000 -146.0000 52

 11 omega   56.00  103.00   1.0000   27.5700
omega____ theta____ kappa____ phi______ frames
    -       12.8029  179.0000   30.0000 47

 12 omega   56.00  103.00   1.0000   27.5700
omega____ theta____ kappa____ phi______ frames
    -       12.8029  179.0000  150.0000 47

 13 omega  -14.00   89.00   1.0000   27.5700
omega____ theta____ kappa____ phi______ frames
    -       12.8029   38.0000   60.0000 103

 14 omega  -14.00   52.00   1.0000   27.5700
omega____ theta____ kappa____ phi______ frames
    -       12.8029   38.0000  120.0000 66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0325717000
_diffrn_orient_matrix_UB_12      0.0382937000
_diffrn_orient_matrix_UB_13      -0.0078480000
_diffrn_orient_matrix_UB_21      -0.0272350000
_diffrn_orient_matrix_UB_22      -0.0104192000
_diffrn_orient_matrix_UB_23      -0.0404743000
_diffrn_orient_matrix_UB_31      -0.0973994000
_diffrn_orient_matrix_UB_32      -0.0098874000
_diffrn_orient_matrix_UB_33      0.0121835000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            53889
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.737
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.297
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.1806
_exptl_crystal_size_mid          0.1515
_exptl_crystal_size_min          0.1108
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3898
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.286
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0186
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.4723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0548
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3473
_reflns_number_total             3898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05584c2.cif
_cod_data_source_block           gilr1
_cod_depositor_comments
;Adding full bibliography for 7059197--7059199.cif.

 Adding full bibliography for 7059197--7059199.cif.
;
_cod_database_code               7059199
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C24 H44 N8 O22 Cu4'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups, All O(H,H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1W-H1WA
 0.85 with sigma of 0.001
 H4WA-H4WB
 1.34 with sigma of 0.02
 H4A-N4 = H4B-N4
 1 with sigma of 0.01
 H3A-N3 = H3B-N3
 1 with sigma of 0.01
 O1W-H1WB
 0.85 with sigma of 0.001
 O4W-H4WA = O4W-H4WB
 0.85 with sigma of 0.001
3.a Free rotating group:
 O3W(H3WA,H3WB), O5W(H5WA,H5WB), O2W(H2WA,H2WB), O4W(H1WB,H4A,H3A,H4B,H3B)
3.b Rotating group:
 O1W(H1WA)
3.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C11(H11A,H11B)
3.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C7(H7), C9(H9)
;
_shelx_res_checksum              47196
_olex2_submission_special_instructions 'No special instructions were received'