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_7239916
_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 N6 O15 Tb2), 0.5(H4 O2)'
_chemical_formula_sum            'C144 H98 N24 O61 Tb8'
_chemical_formula_weight         4411.82
_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                 107.756(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.3527(3)
_cell_length_b                   18.2613(3)
_cell_length_c                   23.1008(4)
_cell_measurement_reflns_used    30336
_cell_measurement_temperature    296.8(4)
_cell_measurement_theta_max      26.4720
_cell_measurement_theta_min      3.6880
_cell_volume                     7775.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.8(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -36.00  58.00   1.00    8.41    --   -9.62  77.00   0.00   94
  2  \w    -61.00  16.00   1.00    8.41    --   -9.62 -77.00  60.00   77
  3  \w    -18.00  10.00   1.00    8.41    --   -9.62 -99.00-120.00   28
  4  \w     -6.00  68.00   1.00    8.41    --   10.64  57.00 -30.00   74
  5  \w    -20.00  20.00   1.00    8.41    --   10.64 -99.00  60.00   40
  6  \w     50.00  77.00   1.00    8.41    --   10.64  57.00-120.00   27
  7  \w    -12.00  14.00   1.00    8.41    --   10.64 -57.00  90.00   26
  8  \w     -6.00  34.00   1.00    8.41    --   10.64  57.00 -90.00   40
  9  \w    -33.00  30.00   1.00    8.41    --   10.64 -38.00 120.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0022252000
_diffrn_orient_matrix_UB_12      0.0375228000
_diffrn_orient_matrix_UB_13      -0.0071832000
_diffrn_orient_matrix_UB_21      -0.0194174000
_diffrn_orient_matrix_UB_22      0.0095693000
_diffrn_orient_matrix_UB_23      0.0204396000
_diffrn_orient_matrix_UB_31      0.0331519000
_diffrn_orient_matrix_UB_32      0.0030797000
_diffrn_orient_matrix_UB_33      0.0238745000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            70994
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.286
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.688
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_description       flake
_exptl_crystal_F_000             4276
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.765
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1077
_refine_ls_number_reflns         13407
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+10.1610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11722
_reflns_number_total             13407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra10975g2.cif
_cod_data_source_block           lrf-l4-zn-tb_sq
_cod_depositor_comments
'Adding full bibliography for 7239914--7239916.cif.'
_cod_database_code               7239916
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.687
_shelx_estimated_absorpt_t_min   0.526
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     23.21
_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
 H21-H31A
 2.2 with sigma of 0.02
 H2_$1-H30A_$2
 2.2 with sigma of 0.02
3. Rigid bond restraints
 O17, O22, O21, O7, O11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C27, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O29 \\sim O26 \\sim O24 \\sim O17 \\sim O22 \\sim O21 \\sim O5 \\sim O4 \\sim
O7 \\sim O14 \\sim O11: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C27 \\sim C28: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
5. Others
 Fixed Sof: H1A(0.5) H1B(0.5)
6.a Free rotating group:
 O1(H1A,H1B)
6.b Rotating group:
 O30(H30A,H30B), O29(H29A,H29B), O31(H31A,H31B), O15(H15A,H15B), O14(H14A,
 H14B), O16(H16A,H16B)
6.c Aromatic/amide H refined with riding coordinates:
 C38(H38), C39(H39), C40(H40), C43(H43), C44(H44), C45(H45), C50(H50),
 C51(H51), C52(H52), C55(H55), C56(H56), C57(H57), C62(H62), C63(H63), C64(H64),
  C67(H67), C68(H68), C69(H69), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C26(H26), C27(H27),
  C28(H28), C31(H31), C32(H32), C33(H33)
;
_shelx_res_checksum              55497
_shelx_fab_checksum              54373
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.757
_oxdiff_exptl_absorpt_empirical_full_min 0.693