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#$Date: 2024-10-06 11:00:42 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295251 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/66/7716653.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_7716653
loop_
_publ_author_name
'da Silveira, Cleverton O. C.'
'Oliveira, Willian X. C.'
'da Silva Júnior, Eufrânio N'
'Alvarenga, Meiry E.'
'Martins, Felipe T.'
'Gatto, Claudia C.'
'Pinheiro, Carlos B.'
'Pedroso, Emerson F.'
'Silva, Júlia P O'
'Marques, Lippy F.'
'Santos, Moliria V.'
'Torres, Francisco R.'
'Euclides, Rividy'
'Freire, Ricardo O.'
'Nunes, Wallace C.'
'de Almeida, Adriele A.'
'Knobel, Marcelo'
'Pereira, Cynthia L. M.'
_publ_section_title
;
 Photoluminescence and magnetic properties of isostructural europium(III),
 gadolinium(III) and terbium(III) oxamate-based coordination polymers.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14995
_journal_page_last               15009
_journal_paper_doi               10.1039/d4dt01290a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_sum            'C28 H32 Gd N3 O12 S2'
_chemical_formula_weight         823.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-03-19 deposited with the CCDC.	2024-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.1110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6449(2)
_cell_length_b                   9.41980(10)
_cell_length_c                   21.9157(2)
_cell_measurement_reflns_used    24549
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      78.5340
_cell_measurement_theta_min      2.9310
_cell_volume                     3284.10(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    Superflip
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            50607
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.249
_diffrn_reflns_theta_min         2.953
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    14.816
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.246
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.041
_refine_diff_density_max         1.564
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         6006
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0325
_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)+(0.0397P)²+4.8925P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5657
_reflns_number_total             6006
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01290a2.cif
_cod_data_source_block           Gdphox
_cod_depositor_comments
'Adding full bibliography for 7716652--7716654.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7716653
_shelx_shelxl_version_number     2018/3
_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Gd1 Gd 0.60336(2) 0.72091(2) 0.23966(2) 0.02316(7) Uani 1 1 d . . . . .
S1 S 0.58550(7) 0.34405(10) 0.21091(5) 0.0470(2) Uani 1 1 d . . . . .
S2 S 0.70062(8) 0.52333(12) 0.38251(5) 0.0527(3) Uani 1 1 d . . . . .
O11 O 0.57171(17) 0.4929(3) 0.18614(13) 0.0373(6) Uani 1 1 d . . . . .
O3 O 0.49159(15) 0.8752(3) 0.17248(11) 0.0346(6) Uani 1 1 d . . . . .
O2 O 0.60131(16) 0.7413(2) 0.12803(11) 0.0293(5) Uani 1 1 d . . . . .
O5 O 0.82800(15) 0.4462(2) 0.27626(11) 0.0315(5) Uani 1 1 d . . . . .
O10 O 0.62851(18) 0.5520(3) 0.32331(13) 0.0420(6) Uani 1 1 d . . . . .
O4 O 0.73746(15) 0.6229(2) 0.23647(11) 0.0308(5) Uani 1 1 d . . . . .
O9 O 0.53830(16) 0.8708(3) 0.30720(13) 0.0398(6) Uani 1 1 d . . . . .
O7 O 0.46542(17) 0.6462(3) 0.24081(14) 0.0412(6) Uani 1 1 d . . . . .
N1 N 0.43121(18) 0.9775(3) 0.07581(14) 0.0302(6) Uani 1 1 d . . . . .
H1 H 0.436026 0.987944 0.038056 0.036 Uiso 1 1 calc R U . . .
O6 O 0.70551(15) 0.8240(2) 0.33606(11) 0.0307(5) Uani 1 1 d . . . . .
O8 O 0.3412(2) 0.7142(4) 0.2506(2) 0.0622(9) Uani 1 1 d . . . . .
N2 N 0.4126(2) 0.9433(4) 0.31911(17) 0.0456(8) Uani 1 1 d . . . . .
H2 H 0.359356 0.928059 0.305884 0.055 Uiso 1 1 calc R U . . .
N3 N 0.78676(18) 1.0109(3) 0.38370(13) 0.0278(6) Uani 1 1 d . . . . .
H3 H 0.808218 1.089739 0.376244 0.033 Uiso 1 1 calc R U . . .
O1 O 0.5590(2) 0.8649(4) 0.03735(15) 0.0594(9) Uani 1 1 d . . . . .
O12 O 0.2693(3) 0.4581(5) 0.2083(3) 0.0893(14) Uani 1 1 d D . . . .
C3 C 0.3624(2) 1.0473(4) 0.08942(16) 0.0299(7) Uani 1 1 d . . . . .
C7 C 0.2663(3) 1.2427(5) 0.0689(2) 0.0484(11) Uani 1 1 d . . . . .
H7 H 0.246557 1.326474 0.047233 0.058 Uiso 1 1 calc R U . . .
C17 C 0.7759(2) 0.5105(3) 0.23242(15) 0.0240(6) Uani 1 1 d . . . . .
C2 C 0.4886(2) 0.8976(3) 0.11644(15) 0.0265(7) Uani 1 1 d . . . . .
C19 C 0.8055(2) 0.9668(4) 0.44843(16) 0.0311(7) Uani 1 1 d . . . . .
C24 C 0.8845(3) 0.9945(4) 0.48911(19) 0.0407(9) Uani 1 1 d . . . . .
H24 H 0.924508 1.039639 0.473946 0.049 Uiso 1 1 calc R U . . .
C8 C 0.3341(2) 1.1734(4) 0.05796(19) 0.0373(8) Uani 1 1 d . . . . .
H8 H 0.360512 1.211331 0.029668 0.045 Uiso 1 1 calc R U . . .
C1 C 0.5557(2) 0.8299(4) 0.09010(16) 0.0302(7) Uani 1 1 d . . . . .
C26 C 0.5759(3) 0.2359(4) 0.1429(3) 0.0558(12) Uani 1 1 d . . . . .
H26A H 0.584172 0.138269 0.155755 0.084 Uiso 1 1 calc R U . . .
H26B H 0.520841 0.247515 0.113342 0.084 Uiso 1 1 calc R U . . .
H26C H 0.617478 0.263393 0.122701 0.084 Uiso 1 1 calc R U . . .
C4 C 0.3234(3) 0.9919(5) 0.1317(2) 0.0440(9) Uani 1 1 d . . . . .
H4 H 0.341535 0.906428 0.152453 0.053 Uiso 1 1 calc R U . . .
C9 C 0.4171(3) 0.7272(4) 0.2593(2) 0.0385(9) Uani 1 1 d . . . . .
C27 C 0.6565(5) 0.5456(7) 0.4464(3) 0.0842(19) Uani 1 1 d . . . . .
H27A H 0.698956 0.528937 0.486164 0.126 Uiso 1 1 calc R U . . .
H27B H 0.635461 0.640611 0.445735 0.126 Uiso 1 1 calc R U . . .
H27C H 0.611345 0.479281 0.441748 0.126 Uiso 1 1 calc R U . . .
C18 C 0.7387(2) 0.9401(3) 0.33382(15) 0.0245(7) Uani 1 1 d . . . . .
C10 C 0.4616(2) 0.8562(4) 0.29758(18) 0.0361(8) Uani 1 1 d . . . . .
C23 C 0.9040(3) 0.9549(5) 0.5525(2) 0.0510(11) Uani 1 1 d . . . . .
H23 H 0.957452 0.972949 0.579710 0.061 Uiso 1 1 calc R U . . .
C6 C 0.2283(3) 1.1895(5) 0.1111(2) 0.0546(12) Uani 1 1 d . . . . .
H6 H 0.183068 1.237121 0.118423 0.066 Uiso 1 1 calc R U . . .
C20 C 0.7455(3) 0.9023(5) 0.4716(2) 0.0476(10) Uani 1 1 d . . . . .
H20 H 0.691669 0.885511 0.444692 0.057 Uiso 1 1 calc R U . . .
C25 C 0.4913(5) 0.2931(7) 0.2272(4) 0.099(3) Uani 1 1 d . . . . .
H25A H 0.496781 0.197694 0.243286 0.148 Uiso 1 1 calc R U . . .
H25B H 0.480772 0.356053 0.258386 0.148 Uiso 1 1 calc R U . . .
H25C H 0.445315 0.297886 0.188581 0.148 Uiso 1 1 calc R U . . .
C5 C 0.2572(3) 1.0645(6) 0.1429(2) 0.0568(12) Uani 1 1 d . . . . .
H5 H 0.231713 1.029009 0.172274 0.068 Uiso 1 1 calc R U . . .
C11 C 0.4404(3) 1.0581(5) 0.3616(2) 0.0517(11) Uani 1 1 d . . . . .
C22 C 0.8459(4) 0.8895(5) 0.5756(2) 0.0578(13) Uani 1 1 d . . . . .
H22 H 0.859650 0.863141 0.618371 0.069 Uiso 1 1 calc R U . . .
C21 C 0.7666(4) 0.8630(6) 0.5353(2) 0.0633(14) Uani 1 1 d . . . . .
H21 H 0.726956 0.818260 0.550935 0.076 Uiso 1 1 calc R U . . .
C28 C 0.7082(4) 0.3340(5) 0.3842(2) 0.0658(15) Uani 1 1 d . . . . .
H28A H 0.753025 0.305042 0.420718 0.099 Uiso 1 1 calc R U . . .
H28B H 0.656187 0.294039 0.386691 0.099 Uiso 1 1 calc R U . . .
H28C H 0.719350 0.301263 0.345986 0.099 Uiso 1 1 calc R U . . .
C16 C 0.5114(4) 1.0479(7) 0.4125(3) 0.0825(19) Uani 1 1 d . . . . .
H16 H 0.544188 0.966302 0.417899 0.099 Uiso 1 1 calc R U . . .
C12 C 0.3915(5) 1.1799(7) 0.3542(4) 0.089(2) Uani 1 1 d . . . . .
H12 H 0.343125 1.189976 0.319914 0.107 Uiso 1 1 calc R U . . .
C13 C 0.4172(7) 1.2860(8) 0.3996(6) 0.122(4) Uani 1 1 d . . . . .
H13 H 0.384709 1.367860 0.395226 0.147 Uiso 1 1 calc R U . . .
C14 C 0.4866(7) 1.2761(10) 0.4494(6) 0.127(4) Uani 1 1 d . . . . .
H14 H 0.501741 1.349074 0.479158 0.152 Uiso 1 1 calc R U . . .
C15 C 0.5345(6) 1.1573(10) 0.4556(5) 0.119(3) Uani 1 1 d . . . . .
H15 H 0.583577 1.149870 0.489402 0.143 Uiso 1 1 calc R U . . .
H12A H 0.301(4) 0.549(4) 0.221(5) 0.178 Uiso 1 1 d D U . . .
H12B H 0.309(4) 0.381(6) 0.205(5) 0.178 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
O10 Gd1 O7 75.39(10) . . ?
O10 Gd1 O11 75.16(9) . . ?
O7 Gd1 O11 71.02(9) . . ?
O10 Gd1 O4 79.23(9) . . ?
O7 Gd1 O4 140.73(9) . . ?
O11 Gd1 O4 73.83(8) . . ?
O10 Gd1 O2 140.76(9) . . ?
O7 Gd1 O2 107.51(9) . . ?
O11 Gd1 O2 69.47(8) . . ?
O4 Gd1 O2 75.17(8) . . ?
O10 Gd1 O3 141.71(9) . . ?
O7 Gd1 O3 68.03(9) . . ?
O11 Gd1 O3 102.33(9) . . ?
O4 Gd1 O3 137.74(8) . . ?
O2 Gd1 O3 64.65(8) . . ?
O10 Gd1 O5 134.31(8) . 2_655 ?
O7 Gd1 O5 136.93(9) . 2_655 ?
O11 Gd1 O5 136.99(9) . 2_655 ?
O4 Gd1 O5 81.75(8) . 2_655 ?
O2 Gd1 O5 70.35(8) . 2_655 ?
O3 Gd1 O5 73.21(8) . 2_655 ?
O10 Gd1 O6 71.56(8) . . ?
O7 Gd1 O6 121.38(9) . . ?
O11 Gd1 O6 138.79(8) . . ?
O4 Gd1 O6 76.64(8) . . ?
O2 Gd1 O6 128.64(8) . . ?
O3 Gd1 O6 118.85(8) . . ?
O5 Gd1 O6 63.76(7) 2_655 . ?
O10 Gd1 O9 85.98(10) . . ?
O7 Gd1 O9 65.17(9) . . ?
O11 Gd1 O9 135.40(9) . . ?
O4 Gd1 O9 142.02(8) . . ?
O2 Gd1 O9 131.65(8) . . ?
O3 Gd1 O9 68.99(9) . . ?
O5 Gd1 O9 84.16(9) 2_655 . ?
O6 Gd1 O9 65.49(8) . . ?
O11 S1 C26 105.5(2) . . ?
O11 S1 C25 106.0(3) . . ?
C26 S1 C25 98.4(3) . . ?
O10 S2 C27 104.4(3) . . ?
O10 S2 C28 103.3(2) . . ?
C27 S2 C28 98.3(3) . . ?
S1 O11 Gd1 131.67(15) . . ?
C2 O3 Gd1 119.7(2) . . ?
C1 O2 Gd1 122.7(2) . . ?
C17 O5 Gd1 123.5(2) . 2_645 ?
S2 O10 Gd1 134.40(16) . . ?
C17 O4 Gd1 144.4(2) . . ?
C10 O9 Gd1 116.0(2) . . ?
C9 O7 Gd1 121.9(2) . . ?
C2 N1 C3 125.7(3) . . ?
C18 O6 Gd1 121.0(2) . . ?
C10 N2 C11 126.0(4) . . ?
C18 N3 C19 125.2(3) . . ?
C4 C3 C8 120.0(4) . . ?
C4 C3 N1 122.1(3) . . ?
C8 C3 N1 117.9(3) . . ?
C6 C7 C8 120.7(4) . . ?
O5 C17 O4 127.6(3) . . ?
O5 C17 C18 113.4(3) . 2_645 ?
O4 C17 C18 119.0(3) . 2_645 ?
O3 C2 N1 125.0(3) . . ?
O3 C2 C1 118.8(3) . . ?
N1 C2 C1 116.2(3) . . ?
C24 C19 C20 119.9(4) . . ?
C24 C19 N3 118.5(3) . . ?
C20 C19 N3 121.5(3) . . ?
C19 C24 C23 119.7(4) . . ?
C3 C8 C7 119.5(4) . . ?
O1 C1 O2 128.2(3) . . ?
O1 C1 C2 118.9(3) . . ?
O2 C1 C2 112.9(3) . . ?
C5 C4 C3 119.3(4) . . ?
O8 C9 O7 128.0(4) . . ?
O8 C9 C10 118.3(4) . . ?
O7 C9 C10 113.8(3) . . ?
O6 C18 N3 125.5(3) . . ?
O6 C18 C17 117.9(3) . 2_655 ?
N3 C18 C17 116.5(3) . 2_655 ?
O9 C10 N2 125.2(4) . . ?
O9 C10 C9 119.3(3) . . ?
N2 C10 C9 115.5(3) . . ?
C22 C23 C24 120.9(4) . . ?
C7 C6 C5 119.7(4) . . ?
C21 C20 C19 119.3(4) . . ?
C4 C5 C6 120.7(4) . . ?
C16 C11 C12 119.3(6) . . ?
C16 C11 N2 121.3(4) . . ?
C12 C11 N2 119.2(5) . . ?
C23 C22 C21 119.5(4) . . ?
C22 C21 C20 120.6(5) . . ?
C11 C16 C15 120.5(7) . . ?
C13 C12 C11 117.7(8) . . ?
C14 C13 C12 123.0(8) . . ?
C13 C14 C15 118.7(8) . . ?
C14 C15 C16 120.8(9) . . ?
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
Gd1 O10 2.370(2) . ?
Gd1 O7 2.409(3) . ?
Gd1 O11 2.429(2) . ?
Gd1 O4 2.435(2) . ?
Gd1 O2 2.444(2) . ?
Gd1 O3 2.476(2) . ?
Gd1 O5 2.483(2) 2_655 ?
Gd1 O6 2.487(2) . ?
Gd1 O9 2.510(3) . ?
S1 O11 1.497(3) . ?
S1 C26 1.774(5) . ?
S1 C25 1.773(7) . ?
S2 O10 1.510(3) . ?
S2 C27 1.773(6) . ?
S2 C28 1.787(5) . ?
O3 C2 1.233(4) . ?
O2 C1 1.261(4) . ?
O5 C17 1.245(4) . ?
O4 C17 1.254(4) . ?
O9 C10 1.238(5) . ?
O7 C9 1.260(5) . ?
N1 C2 1.331(4) . ?
N1 C3 1.426(5) . ?
O6 C18 1.233(4) . ?
O8 C9 1.226(5) . ?
N2 C10 1.337(5) . ?
N2 C11 1.414(6) . ?
N3 C18 1.329(4) . ?
N3 C19 1.422(4) . ?
O1 C1 1.219(4) . ?
C3 C4 1.382(5) . ?
C3 C8 1.384(5) . ?
C7 C6 1.360(7) . ?
C7 C8 1.385(6) . ?
C17 C18 1.549(4) 2_645 ?
C2 C1 1.538(5) . ?
C19 C24 1.379(5) . ?
C19 C20 1.387(6) . ?
C24 C23 1.381(6) . ?
C4 C5 1.379(6) . ?
C9 C10 1.537(6) . ?
C23 C22 1.364(7) . ?
C6 C5 1.381(7) . ?
C20 C21 1.385(6) . ?
C11 C16 1.368(8) . ?
C11 C12 1.389(8) . ?
C22 C21 1.378(8) . ?
C16 C15 1.375(9) . ?
C12 C13 1.386(12) . ?
C13 C14 1.340(15) . ?
C14 C15 1.357(14) . ?
