The coordination chemistry of benzhydrazide with lanthanide(iii) ions: hydrothermal in situ ligand formation, structures, magnetic and photoluminescence sensing properties
Theppitak, Chatphorn; Kielar, Filip; Dungkaew, Winya; Sukwattanasinitt, Mongkol; Kangkaew, Laongdao; Sahasithiwat, Somboon; Zenno, Hikaru; Hayami, Shinya; Chainok, Kittipong; RSC Advances 11 (2021) 24709–24721; doi:10.1039/D1RA03106F

data_7243206
_publ_section_title
;
 The coordination chemistry of benzhydrazide with lanthanide(iii) ions:
 hydrothermal in situ ligand formation, structures, magnetic and
 photoluminescence sensing properties
;
_journal_issue                   40
_journal_name_full               'RSC Advances'
_journal_page_first              24709
_journal_page_last               24721
_journal_paper_doi               10.1039/D1RA03106F
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C28 H32 N9 O7 Sm, 3(N O3)'
_chemical_formula_sum            'C28 H32 N12 O16 Sm'
_chemical_formula_weight         943.00
_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     dual
_audit_creation_date             2021-02-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-02-21 deposited with the CCDC.	2021-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.982(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.726(8)
_cell_length_b                   15.346(5)
_cell_length_c                   10.498(3)
_cell_measurement_reflns_used    4334
_cell_measurement_temperature    296
_cell_measurement_theta_max      24.104
_cell_measurement_theta_min      3.139
_cell_volume                     3923(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.0
_diffrn_detector                 'Bruker PHOTON 200 area detector'
_diffrn_detector_area_resol_mean 7.39
_diffrn_detector_type            'PHOTON II area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'BRUKER D8 QUEST CMOS PHOTON II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13754
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.400
_diffrn_reflns_theta_min         3.138
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.580
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0617 before and 0.0517 after correction. The Ratio of minimum to maximum transmission is 0.8861. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.744
_refine_diff_density_min         -1.469
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         3593
_refine_ls_number_restraints     325
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0493P)^2^+7.2731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2853
_reflns_number_total             3593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra03106f2.cif
_cod_data_source_block           1sm
_cod_database_code               7243206
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.722
_shelx_estimated_absorpt_t_min   0.649
_olex2_refinement_description
;
1. Restrained distances
 N4-H4 = N2-H2
 0.86 with sigma of 0.01
 N3-H3A = N3-H3B = N1-H1B = N1-H1A
 0.89 with sigma of 0.01
 N5-O3 \\sim N5-O5 \\sim N5-O4
 with sigma of 0.02
 O10-O11 \\sim O10-O9
 with sigma of 0.01
 O11-O9 \\sim O11-O10
 with sigma of 0.01
 N7-O9 \\sim N7-O10 \\sim N7-O11
 with sigma of 0.02
 O9-O10 \\sim O9-O11
 with sigma of 0.01
 C2-C3 \\sim C2A-C3A
 with sigma of 0.02
 C2-C4 \\sim C2A-C4A
 with sigma of 0.04
 C2-C7 \\sim C2A-C7A
 with sigma of 0.02
 C3-C4 \\sim C3A-C4A
 with sigma of 0.02
 C3-C5 \\sim C3A-C5A
 with sigma of 0.04
 C2-C6 \\sim C2A-C6A
 with sigma of 0.04
 C3-C7 \\sim C3A-C7A
 with sigma of 0.04
 C4-C6 \\sim C4A-C6A
 with sigma of 0.04
 C5-C7 \\sim C5A-C7A
 with sigma of 0.04
 C4-C5 \\sim C4A-C5A
 with sigma of 0.02
 C1-C2 \\sim C1-C2A
 with sigma of 0.02
 C5-C6 \\sim C5A-C6A
 with sigma of 0.02
 C6-C7 \\sim C6A-C7A
 with sigma of 0.02
 C1-C3 \\sim C1-C3A
 with sigma of 0.04
 C1-C7 \\sim C1-C7A
 with sigma of 0.04
 O6-O7 \\sim O6A-O7A
 with sigma of 0.04
 O8-N6 \\sim O8A-N6A
 with sigma of 0.02
 O6-O8 \\sim O6A-O8A
 with sigma of 0.04
 O7-O8 \\sim O7A-O8A
 with sigma of 0.04
 O7-N6 \\sim O7A-N6A
 with sigma of 0.02
 O6-N6 \\sim O6A-N6A
 with sigma of 0.02
2. Restrained planarity
 O9, O10, O11, N7
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(N7) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2A) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C5A)
\\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C3A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N6) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N6A) \\sim Ueq, Uanis(O6A) \\sim Ueq, Uanis(O7A) \\sim Ueq, Uanis(O8A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O9, O10, O11, N7
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C1, C2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1, C2A, C3A, C4A, C5A, C6A, C7A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O6, O7, O8, N6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O6A, O7A, O8A, N6A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C2A)=Sof(C3A)=Sof(H3AA)=Sof(C4A)=Sof(H4AA)=Sof(C5A)=Sof(H5A)=Sof(C6A)=
 Sof(H6A)=Sof(C7A)=Sof(H7A)=1-FVAR(1)
 Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4A)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=
 Sof(C7)=Sof(H7)=FVAR(1)
 Sof(O6A)=Sof(O7A)=Sof(O8A)=Sof(N6A)=1-FVAR(2)
 Sof(O6)=Sof(O7)=Sof(O8)=Sof(N6)=FVAR(2)
 Fixed Sof: O3(0.5) O4(0.5) O5(0.5) O9(0.5) O10(0.5) O11(0.5) N5(0.5) N7(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C3A(H3AA), C4(H4A), C4A(H4AA), C5(H5), C5A(H5A), C6(H6), C6A(H6A),
 C7(H7), C7A(H7A), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14)
;
_shelx_res_checksum              38283
_olex2_submission_special_instructions 'No special instructions were received'