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#$Date: 2021-04-05 17:35:19 +0300 (Mon, 05 Apr 2021) $
#$Revision: 263730 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/21/7242174.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7242174
loop_
_publ_author_name
'da Cunha, Tamyris T.'
'da Silveira, Cleverton O. C.'
'Barbosa, Vitor M. M.'
'Oliveira, Willian X. C.'
'da Silva Júnior, Eufrânio N.'
'Ferreira, Fabio F.'
'Pedroso, Emerson F.'
'Pereira, Cynthia L. M.'
_publ_section_title
;
 Ferromagnetic coupling in a dicopper(ii) oxamate complex bridged by
 carboxylate groups
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1885
_journal_page_last               1897
_journal_paper_doi               10.1039/D0CE01742F
_journal_volume                  23
_journal_year                    2021
_chemical_formula_sum            'C32 H32 Cu2 N4 O20'
_chemical_formula_weight         919.72
_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_method           SHELXL-2014/7
_audit_update_record
;
2020-11-09 deposited with the CCDC.	2021-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                67.684(6)
_cell_angle_beta                 74.454(6)
_cell_angle_gamma                65.499(6)
_cell_formula_units_Z            1
_cell_length_a                   8.7512(6)
_cell_length_b                   9.7054(6)
_cell_length_c                   12.4718(9)
_cell_measurement_reflns_used    4018
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.3950
_cell_measurement_theta_min      2.8850
_cell_volume                     883.98(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    Superflip
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4186
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10811
_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         26.371
_diffrn_reflns_theta_min         2.423
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_correction_T_min  0.769
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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            'light green'
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_description       block
_exptl_crystal_F_000             470
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.128
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3615
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0333
_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/[σ²(Fo²)+(0.0351P)²+0.4059P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3075
_reflns_number_total             3615
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01742f2.cif
_cod_data_source_block           Cu2(H2O)2L4
_cod_depositor_comments
'Adding full bibliography for 7242174--7242176.cif.'
_cod_database_code               7242174
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4074(3) 0.8518(3) 0.48478(19) 0.0121(5) Uani 1 1 d . . . . .
C2 C 0.5256(3) 0.9197(3) 0.38050(19) 0.0115(5) Uani 1 1 d . . . . .
C3 C 0.5538(3) 1.1670(3) 0.23492(19) 0.0126(5) Uani 1 1 d . . . . .
C4 C 0.4842(3) 1.3308(3) 0.2135(2) 0.0153(5) Uani 1 1 d . . . . .
H4 H 0.3803 1.3764 0.2571 0.018 Uiso 1 1 calc R U . . .
C5 C 0.5666(3) 1.4272(3) 0.1287(2) 0.0167(5) Uani 1 1 d . . . . .
H5 H 0.5198 1.5391 0.1143 0.020 Uiso 1 1 calc R U . . .
C6 C 0.7173(3) 1.3604(3) 0.0648(2) 0.0151(5) Uani 1 1 d . . . . .
C7 C 0.7839(3) 1.1971(3) 0.0827(2) 0.0160(5) Uani 1 1 d . . . . .
H7 H 0.8852 1.1524 0.0366 0.019 Uiso 1 1 calc R U . . .
C8 C 0.7023(3) 1.0995(3) 0.1681(2) 0.0160(5) Uani 1 1 d . . . . .
H8 H 0.7473 0.9879 0.1807 0.019 Uiso 1 1 calc R U . . .
C9 C 1.0113(3) 0.3789(3) 0.44181(19) 0.0108(5) Uani 1 1 d . . . . .
C10 C 0.9004(3) 0.3065(3) 0.54875(19) 0.0116(5) Uani 1 1 d . . . . .
C11 C 0.8965(3) 0.0585(3) 0.7045(2) 0.0126(5) Uani 1 1 d . . . . .
C12 C 0.9482(3) -0.1010(3) 0.7142(2) 0.0153(5) Uani 1 1 d . . . . .
H12 H 1.0296 -0.1416 0.6557 0.018 Uiso 1 1 calc R U . . .
C13 C 0.8811(3) -0.2013(3) 0.8094(2) 0.0165(5) Uani 1 1 d . . . . .
H13 H 0.9167 -0.3107 0.8163 0.020 Uiso 1 1 calc R U . . .
C14 C 0.7623(3) -0.1416(3) 0.8943(2) 0.0155(5) Uani 1 1 d . . . . .
C15 C 0.7115(3) 0.0178(3) 0.8855(2) 0.0182(5) Uani 1 1 d . . . . .
H15 H 0.6304 0.0581 0.9442 0.022 Uiso 1 1 calc R U . . .
C16 C 0.7792(3) 0.1182(3) 0.7906(2) 0.0171(5) Uani 1 1 d . . . . .
H16 H 0.7455 0.2270 0.7846 0.020 Uiso 1 1 calc R U . . .
N1 N 0.4666(2) 1.0744(2) 0.32805(16) 0.0119(4) Uani 1 1 d . . . . .
H1 H 0.3619 1.1262 0.3532 0.014 Uiso 1 1 calc R U . . .
N2 N 0.9712(2) 0.1555(2) 0.60531(16) 0.0122(4) Uani 1 1 d . . . . .
H2 H 1.0771 0.1087 0.5790 0.015 Uiso 1 1 calc R U . . .
O1 O 0.2673(2) 0.9376(2) 0.51413(14) 0.0176(4) Uani 1 1 d . . . . .
O2 O 0.47641(19) 0.70163(18) 0.53194(13) 0.0133(3) Uani 1 1 d . . . . .
O3 O 0.6680(2) 0.82629(19) 0.35354(14) 0.0149(4) Uani 1 1 d . . . . .
O4 O 0.7967(2) 1.4602(2) -0.01553(14) 0.0219(4) Uani 1 1 d . . . . .
H4A H 0.8863 1.4071 -0.0489 0.033 Uiso 1 1 calc R U . . .
O5 O 1.1596(2) 0.30091(19) 0.41866(14) 0.0151(4) Uani 1 1 d . . . . .
O6 O 0.93133(19) 0.52334(18) 0.38714(13) 0.0126(3) Uani 1 1 d . . . . .
O7 O 0.7521(2) 0.39457(19) 0.57429(14) 0.0135(3) Uani 1 1 d . . . . .
O8 O 0.6933(2) -0.2361(2) 0.99049(14) 0.0212(4) Uani 1 1 d . . . . .
H8A H 0.7345 -0.3298 0.9876 0.032 Uiso 1 1 calc R U . . .
O9 O 0.6084(2) 0.5616(2) 0.32362(15) 0.0207(4) Uani 1 1 d D . . . .
O10 O 0.9365(2) 0.6826(2) 0.14313(16) 0.0265(5) Uani 1 1 d D . . . .
Cu1 Cu 0.69953(3) 0.60815(3) 0.45616(2) 0.01239(10) Uani 1 1 d . . . . .
H9A H 0.502(2) 0.621(3) 0.324(2) 0.019 Uiso 1 1 d D U . . .
H9B H 0.612(3) 0.467(2) 0.347(2) 0.019 Uiso 1 1 d D U . . .
H10A H 0.847(3) 0.694(3) 0.123(2) 0.019 Uiso 1 1 d D U . . .
H10B H 0.937(3) 0.634(3) 0.2144(15) 0.019 Uiso 1 1 d D U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 O2 127.1(2) . . ?
O1 C1 C2 120.9(2) . . ?
O2 C1 C2 111.96(19) . . ?
O3 C2 N1 125.4(2) . . ?
O3 C2 C1 118.4(2) . . ?
N1 C2 C1 116.3(2) . . ?
C4 C3 C8 120.5(2) . . ?
C4 C3 N1 116.7(2) . . ?
C8 C3 N1 122.8(2) . . ?
C5 C4 C3 119.9(2) . . ?
C6 C5 C4 119.9(2) . . ?
O4 C6 C5 117.7(2) . . ?
O4 C6 C7 121.9(2) . . ?
C5 C6 C7 120.4(2) . . ?
C8 C7 C6 120.0(2) . . ?
C7 C8 C3 119.3(2) . . ?
O5 C9 O6 127.0(2) . . ?
O5 C9 C10 120.5(2) . . ?
O6 C9 C10 112.54(19) . . ?
O7 C10 N2 125.7(2) . . ?
O7 C10 C9 118.3(2) . . ?
N2 C10 C9 116.0(2) . . ?
C12 C11 C16 120.3(2) . . ?
C12 C11 N2 117.5(2) . . ?
C16 C11 N2 122.2(2) . . ?
C11 C12 C13 120.0(2) . . ?
C14 C13 C12 119.8(2) . . ?
O8 C14 C13 122.0(2) . . ?
O8 C14 C15 117.6(2) . . ?
C13 C14 C15 120.4(2) . . ?
C16 C15 C14 119.9(2) . . ?
C15 C16 C11 119.6(2) . . ?
C2 N1 C3 127.2(2) . . ?
C10 N2 C11 127.6(2) . . ?
C1 O2 Cu1 114.19(14) . . ?
C2 O3 Cu1 110.77(14) . . ?
C9 O6 Cu1 114.40(14) . . ?
C10 O7 Cu1 110.33(14) . . ?
O2 Cu1 O6 174.53(7) . . ?
O2 Cu1 O3 84.68(7) . . ?
O6 Cu1 O3 93.77(7) . . ?
O2 Cu1 O7 96.38(7) . . ?
O6 Cu1 O7 84.29(6) . . ?
O3 Cu1 O7 170.58(7) . . ?
O2 Cu1 O9 95.47(7) . . ?
O6 Cu1 O9 89.76(7) . . ?
O3 Cu1 O9 89.78(7) . . ?
O7 Cu1 O9 99.42(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.214(3) . ?
C1 O2 1.282(3) . ?
C1 C2 1.546(3) . ?
C2 O3 1.248(3) . ?
C2 N1 1.319(3) . ?
C3 C4 1.389(3) . ?
C3 C8 1.394(3) . ?
C3 N1 1.429(3) . ?
C4 C5 1.384(3) . ?
C5 C6 1.383(3) . ?
C6 O4 1.369(3) . ?
C6 C7 1.391(3) . ?
C7 C8 1.389(3) . ?
C9 O5 1.221(3) . ?
C9 O6 1.279(3) . ?
C9 C10 1.541(3) . ?
C10 O7 1.258(3) . ?
C10 N2 1.314(3) . ?
C11 C12 1.386(3) . ?
C11 C16 1.390(3) . ?
C11 N2 1.427(3) . ?
C12 C13 1.388(3) . ?
C13 C14 1.383(3) . ?
C14 O8 1.372(3) . ?
C14 C15 1.389(3) . ?
C15 C16 1.388(3) . ?
O2 Cu1 1.9291(16) . ?
O3 Cu1 1.9604(16) . ?
O6 Cu1 1.9366(16) . ?
O7 Cu1 1.9830(15) . ?
O9 Cu1 2.2685(18) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O10 H10B O6 0.833(16) 2.007(17) 2.840(2) 178(3) .
O10 H10A O8 0.837(16) 2.141(19) 2.901(3) 151(2) 1_564
O9 H9B O2 0.842(16) 2.02(2) 2.772(2) 148(3) 2_666
O9 H9A O7 0.867(17) 2.28(2) 2.983(2) 138(2) 2_666
N1 H1 O5 0.88 2.11 2.948(3) 158.2 1_465
N2 H2 O1 0.88 2.05 2.861(3) 153.4 1_645
O8 H8A O4 0.84 1.89 2.726(3) 172.3 1_536
O4 H4A O10 0.84 1.80 2.628(3) 170.1 2_775
N1 H1 O1 0.88 2.38 2.757(2) 106.5 .
N2 H2 O5 0.88 2.35 2.740(2) 107.2 .
