Three series of heterometallic Ni <sup>II</sup> –Ln <sup>III</sup> Schiff base complexes: synthesis, crystal structures and magnetic characterization
Jiang, Lin; Liu, Yue; Liu, Xin; Tian, Jinlei; Yan, Shiping; Dalton Transactions 46 (2017) 12558–12573; doi:10.1039/C7DT02351K

data_1546880
_publ_section_title
;
 Three series of heterometallic Ni <sup>II</sup> --Ln <sup>III</sup>
 Schiff base complexes: synthesis, crystal structures and magnetic
 characterization
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              12558
_journal_page_last               12573
_journal_paper_doi               10.1039/C7DT02351K
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C31 H24 F15 N2 Ni O12 Tb'
_chemical_formula_sum            'C31 H24 F15 N2 Ni O12 Tb'
_chemical_formula_weight         1119.14
_chemical_name_systematic
;
 ? 
;
_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_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-01-02 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.946(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2854(7)
_cell_length_b                   12.6822(4)
_cell_length_c                   16.6662(5)
_cell_measurement_reflns_used    11694
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3827.8(2)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      113
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.9971
_diffrn_measured_fraction_theta_max 0.9971
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9850
              2theta: -15.1058
scan:
    Number of images: 300
               Slice: -105.0000 - 45.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9850
              2theta: -15.1058
scan:
    Number of images: 200
               Slice: -105.0000 - -5.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.9850
              2theta: -15.1058
;
_diffrn_measurement_device
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Pilatus 200K'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.033845
_diffrn_orient_matrix_UB_12      -0.035873
_diffrn_orient_matrix_UB_13      0.035362
_diffrn_orient_matrix_UB_21      -0.064793
_diffrn_orient_matrix_UB_22      -0.039141
_diffrn_orient_matrix_UB_23      0.022309
_diffrn_orient_matrix_UB_31      0.010968
_diffrn_orient_matrix_UB_32      -0.039426
_diffrn_orient_matrix_UB_33      -0.037319
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37786
_diffrn_reflns_theta_full        25.9982
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.03
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.460
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.9418
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       prism
_exptl_crystal_F_000             2194.9558
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.7754
_refine_diff_density_min         -1.0448
_refine_diff_density_rms         0.1805
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             6.7270
_refine_ls_goodness_of_fit_ref   0.9983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    41
_refine_ls_number_parameters     562
_refine_ls_number_reflns         7514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9983
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+64.1247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                7118
_reflns_number_total             7514
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt02351k2.cif
_cod_data_source_block           y
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               1546880
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Rotating group:
 O12(H12a,H12b)
2.b Ternary CH refined with riding coordinates:
 C10(H10)
2.c Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C11(H11a,H11b)
2.d Aromatic/amide H refined with riding coordinates:
 C14(H14), C12(H12), C16(H16), C6(H6), C24(H24), C5(H5), C4(H4), C8(H8),
 C15(H15), C29(H29)
2.e Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C1(H1a,H1b,H1c)
2.f Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'