Lanthanide complexes based on a conjugated pyridine carboxylate ligand: structures, luminescence and magnetic properties
Li, Rong-fang; Li, Rui-hao; Liu, Xin-fang; Chang, Xin-hong; Feng, Xun; RSC Advances 10 (2020) 6192–6199; doi:10.1039/C9RA10975G

data_7239914
_publ_section_title
;
 Lanthanide complexes based on a conjugated pyridine carboxylate ligand:
 structures, luminescence and magnetic properties
;
_journal_issue                   11
_journal_name_full               'RSC Advances'
_journal_page_first              6192
_journal_page_last               6199
_journal_paper_doi               10.1039/C9RA10975G
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         '4(C36 H24 Dy2 N6 O15), 0.5(H4 O2)'
_chemical_formula_sum            'C144 H98 Dy8 N24 O61'
_chemical_formula_weight         4440.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-12-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-01-17 deposited with the CCDC.	2020-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.892(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.329(4)
_cell_length_b                   18.257(4)
_cell_length_c                   23.014(4)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.499
_cell_measurement_theta_min      2.415
_cell_volume                     7729(3)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            48479
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
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_diffrn_reflns_theta_max         28.600
_diffrn_reflns_theta_min         1.107
_exptl_absorpt_coefficient_mu    3.917
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_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_description       flake
_exptl_crystal_F_000             4292
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
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_refine_ls_extinction_method     none
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_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.077
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0895P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14705
_reflns_number_total             19178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra10975g2.cif
_cod_data_source_block           222_sq
_cod_depositor_comments
'Adding full bibliography for 7239914--7239916.cif.'
_cod_original_cell_volume        7728(3)
_cod_database_code               7239914
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.610
_shelx_estimated_absorpt_t_min   0.493
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H21A-O21
 0.82 with sigma of 0.02
 O21-H21B
 0.82 with sigma of 0.02
 H21A-H21B
 1.4 with sigma of 0.02
3. Others
 Fixed Sof: H1A(0.5) H1B(0.5)
4.a Free rotating group:
 O1(H1A,H1B)
4.b Rotating group:
 O22(H22A,H22B), O15(H15A,H15B), O23(H23A,H23B), O16(H16A,H16B), O14(H14A,H14B)
4.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C20(H20), C52(H52), C68(H68), C10(H10), C51(H51), C53(H53),
 C39(H39), C56(H56), C32(H32), C58(H58), C40(H40), C65(H65), C5(H5), C15(H15),
 C69(H69), C27(H27), C28(H28), C64(H64), C17(H17), C46(H46), C33(H33), C29(H29),
  C57(H57), C63(H63), C21(H21), C34(H34), C16(H16), C41(H41), C22(H22),
 C70(H70), C3(H3), C4(H4), C44(H44), C45(H45)
;
_shelx_res_checksum              36975
_shelx_fab_checksum              56523
_olex2_submission_special_instructions 'No special instructions were received'