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_7059197
_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 O8, 1.5(H2 O)'
_chemical_formula_sum            'C13 H19 Cu2 N4 O9.5'
_chemical_formula_weight         510.40
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2019-11-05
_audit_creation_method
;
Olex2 1.3
(compiled Sep 10 2019 10:50:26 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-01-07 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.423(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.475(5)
_cell_length_b                   6.751(5)
_cell_length_c                   25.546(5)
_cell_measurement_reflns_used    6110
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      66.0807
_cell_measurement_theta_min      3.7143
_cell_volume                     3448(3)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector_area_resol_mean 10.4186
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0051367000
_diffrn_orient_matrix_UB_12      -0.0168757000
_diffrn_orient_matrix_UB_13      -0.0584600000
_diffrn_orient_matrix_UB_21      0.0758238000
_diffrn_orient_matrix_UB_22      0.0390983000
_diffrn_orient_matrix_UB_23      0.0264978000
_diffrn_orient_matrix_UB_31      0.0128365000
_diffrn_orient_matrix_UB_32      -0.2240420000
_diffrn_orient_matrix_UB_33      0.0089968000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17648
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.185
_diffrn_reflns_theta_max         66.185
_diffrn_reflns_theta_min         3.717
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.643
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) 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    1.967
_exptl_crystal_description       prism
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         2990
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0569P)^2^+2.5375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2515
_reflns_number_total             2990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05584c2.cif
_cod_data_source_block           cuopcudapoh_4
_cod_depositor_comments
;Adding full bibliography for 7059197--7059199.cif.

 Adding full bibliography for 7059197--7059199.cif.
;
_cod_original_formula_sum        'C13 H19 Cu2 N4 O9.50'
_cod_database_code               7059197
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.611
_shelx_estimated_absorpt_t_min   0.515
_reflns_odcompleteness_completeness 97.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 At 1.5 times of:
  All O(H,H,H,H,H,H) groups
2. Restrained distances
 HW1A-OW1
 0.85 with sigma of 0.02
 OW1-HW1B
 0.85 with sigma of 0.02
 HW2-OW2
 0.85 with sigma of 0.02
 H7A-O7
 0.85 with sigma of 0.02
 HW1B-HW1A
 1.55 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C12(H12)
3.b Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B), C11(H11A,H11B), N3(H3A,H3B), C13(H13A,H13B)
3.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C6(H6), C9(H9), C7(H7)
;
_shelx_res_checksum              68199
_olex2_submission_special_instructions 'No special instructions were received'