A new salicylaldehyde-based azo dye and its two lanthanide(iii) complexes displaying slow magnetic relaxation.
He, Jian-Qiang; Xie, Shang-Fang; Lai, Bi-Lin; Yang, Meng; Chen, Wen-Bin; Zhang, Yi-Quan; Dong, Wen; Dalton transactions (Cambridge, England : 2003) 47 (2018) 14975–14984; doi:10.1039/c8dt02951b

data_7047583
_publ_section_title
;
 A new salicylaldehyde-based azo dye and its two lanthanide(iii) complexes
 displaying slow magnetic relaxation.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14975
_journal_page_last               14984
_journal_paper_doi               10.1039/c8dt02951b
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C30 H28 N15 O11 Tb, C33 H33 N16 O11 Tb'
_chemical_formula_sum            'C63 H91 N31 O37 Tb2'
_chemical_formula_weight         2192.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-13 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.276(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5473(5)
_cell_length_b                   24.3836(7)
_cell_length_c                   20.4332(8)
_cell_measurement_reflns_used    7796
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      71.1540
_cell_measurement_theta_min      3.9590
_cell_volume                     9120.1(5)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.1052
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40060
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.450
_diffrn_reflns_theta_min         3.019
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.409
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.22547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       block
_exptl_crystal_F_000             4448
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.292
_refine_diff_density_min         -1.200
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1054
_refine_ls_number_reflns         17247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1396
_refine_ls_R_factor_gt           0.0941
_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^)+(0.1557P)^2^+72.7190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2552
_refine_ls_wR_factor_ref         0.2923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11098
_reflns_number_total             17247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02951b2.cif
_cod_data_source_block           a_sq_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7047582--7047583.cif.'
_cod_database_code               7047583
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.408
_shelx_estimated_absorpt_t_min   0.284
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1A(0.039) H1B(0.039) H2A(0.043) H2B(0.043) H1(0.035) H6(0.033)
 H11(0.04) H1C(0.041) H4(0.029) H8(0.038) H9(0.045) H10A(0.053) H10B(0.053)
 H10C(0.053) H11A(0.036) H14(0.035) H18(0.029) H19(0.034) H20A(0.075)
 H20B(0.075) H20C(0.075) H21(0.038) H24(0.03) H28(0.025) H29(0.031) H30A(0.045)
 H30B(0.045) H30C(0.045) H12A(0.043) H12B(0.043) H16(0.03) H23(0.044)
 H26(0.038) H31(0.044) H34(0.038) H38(0.032) H39(0.041) H40A(0.057) H40B(0.057)
 H40C(0.057) H41(0.05) H44(0.034) H48(0.028) H49(0.028) H50A(0.07) H50B(0.07)
 H50C(0.07) H51(0.034) H54(0.026) H58(0.024) H59(0.03) H60A(0.041) H60B(0.041)
 H60C(0.041) H61(0.045) H62A(0.079) H62B(0.079) H62C(0.079) H63A(0.069)
 H63B(0.069) H63C(0.069)
 Fixed X: H1A(-0.010501) H1B(0.0329) H2A(-0.1109) H2B(-0.135699) H1(-0.408999)
 H6(0.521301) H11(0.2569) H1C(-0.535501) H4(-0.2729) H8(-0.1993) H9(-0.0793)
 H10A(-0.2548) H10B(-0.217401) H10C(-0.1931) H11A(0.641301) H14(0.279799)
 H18(0.3195) H19(0.2267) H20A(0.1876) H20B(0.1164) H20C(0.187201) H21(0.3494)
 H24(0.282) H28(0.1057) H29(-0.0045) H30A(0.319) H30B(0.3196) H30C(0.311001)
 H12A(0.8524) H12B(0.853101) H16(0.478999) H23(1.1546) H26(0.2315) H31(1.3354)
 H34(0.949499) H38(1.0174) H39(0.8337) H40A(0.9675) H40B(0.9984) H40C(0.936299)
 H41(0.110001) H44(0.472599) H48(0.432099) H49(0.523301) H50A(0.565901)
 H50B(0.6368) H50C(0.565701) H51(0.377) H54(0.4598) H58(0.6362) H59(0.7473)
 H60A(0.4267) H60B(0.4201) H60C(0.431399) H61(0.626801) H62A(0.5804)
 H62B(0.563701) H62C(0.607901) H63A(0.7224) H63B(0.7337) H63C(0.772499)
 Fixed Y: H1A(0.4453) H1B(0.4205) H2A(0.3791) H2B(0.335999) H1(0.4515)
 H6(0.2616) H11(0.0235) H1C(0.4534) H4(0.2758) H8(0.4312) H9(0.4492)
 H10A(0.195201) H10B(0.188001) H10C(0.151201) H11A(0.2235) H14(0.159)
 H18(0.321001) H19(0.385301) H20A(0.106) H20B(0.086399) H20C(0.0994) H21(-
 0.038099) H24(0.2303) H28(0.136) H29(0.173901) H30A(0.3135) H30B(0.3161)
 H30C(0.3702) H12A(0.149301) H12B(0.202) H16(0.503201) H23(0.0752) H26(0.2665)
 H31(0.1569) H34(0.0935) H38(0.2476) H39(0.074699) H40A(0.3336) H40B(0.3318)
 H40C(0.3735) H41(0.301301) H44(0.3697) H48(0.2081) H49(0.1449) H50A(0.4258)
 H50B(0.442499) H50C(0.426499) H51(0.561601) H54(0.2992) H58(0.394)
 H59(0.355801) H60A(0.217) H60B(0.2116) H60C(0.159101) H61(0.121001)
 H62A(0.0051) H62B(0.065701) H62C(0.027) H63A(-0.0129) H63B(0.0055)
 H63C(0.037499)
 Fixed Z: H1A(0.2492) H1B(0.2071) H2A(0.236199) H2B(0.2678) H1(0.487499)
 H6(0.4502) H11(0.151301) H1C(0.501301) H4(0.435399) H8(0.431999) H9(0.413)
 H10A(0.3846) H10B(0.4586) H10C(0.4029) H11A(0.475399) H14(0.388801)
 H18(0.3877) H19(0.3668) H20A(0.3275) H20B(0.353001) H20C(0.4039) H21(0.133101)
 H24(0.1875) H28(0.201) H29(0.222301) H30A(0.1825) H30B(0.259399) H30C(0.2171)
 H12A(0.268301) H12B(0.288301) H16(0.3521) H23(0.008801) H26(0.0431)
 H31(0.0235) H34(0.068201) H38(0.0505) H39(0.091901) H40A(0.031) H40B(0.107201)
 H40C(0.08) H41(0.018701) H44(0.089) H48(0.0945) H49(0.118101) H50A(0.0717)
 H50B(0.1204) H50C(0.148601) H51(0.363701) H54(0.2979) H58(0.2885) H59(0.2668)
 H60A(0.2196) H60B(0.295) H60C(0.2535) H61(0.274499) H62A(0.3097)
 H62B(0.328301) H62C(0.3816) H63A(0.3) H63B(0.374599) H63C(0.3234)
2.a Fitted pentagon refined as free rotating group:
 C2(N1,C1,N2,N3)
;
_shelx_res_checksum              42928
_shelx_fab_checksum              1219
_olex2_submission_special_instructions 'No special instructions were received'