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_1546876
_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         'C64 H53 Eu N2 Ni O11, 2(C H2 Cl2)'
_chemical_formula_sum            'C66 H57 Cl4 Eu N2 Ni O11'
_chemical_formula_weight         1406.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-31
_audit_creation_method
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  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_audit_update_record
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2017-08-14 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                81.784(4)
_cell_angle_beta                 83.709(4)
_cell_angle_gamma                76.878(4)
_cell_formula_units_Z            2
_cell_length_a                   11.2622(8)
_cell_length_b                   12.6894(11)
_cell_length_c                   23.490(2)
_cell_measurement_reflns_used    10062
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3225.4(5)
_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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       -13
_diffrn_reflns_limit_h_min       13
_diffrn_reflns_limit_k_max       -15
_diffrn_reflns_limit_k_min       15
_diffrn_reflns_limit_l_max       -28
_diffrn_reflns_limit_l_min       28
_diffrn_reflns_number            12674
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.038
_exptl_absorpt_coefficient_mu    1.480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   0.744
_exptl_transmission_factor_min   0.698
_refine_diff_density_max         1.931
_refine_diff_density_min         -3.863
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         12498
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_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0620
_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^)+(0.1000P)^2^+30.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1858
_refine_ls_wR_factor_ref         0.1878
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11638
_reflns_number_total             12674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02351k2.cif
_cod_data_source_block           m20160117b_sq_d_sq
_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               1546876
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H32 of C32, H50 of C50, H64 of C64, H37 of C37, H23 of C23, H56 of C56, H47
  of C47, H49 of C49, H54 of C54, H39 of C39, H65 of C65, H8 of C8, H4 of C4,
  H41 of C41, H24 of C24, H55 of C55, H38 of C38, H43 of C43, H6 of C6, H14 of
  C14, H15 of C15, H5 of C5, H46 of C46, H10 of C10, H48 of C48, H31 of C31,
  H61 of C61, {H9A,H9B} of C9, H58 of C58, H12 of C12, H40 of C40, H21 of C21,
  H16 of C16, H35 of C35, H27 of C27, H52 of C52, H53 of C53, H62 of C62, H25
  of C25, {H67A,H67B} of C67, {H11A,H11B} of C11, H33 of C33, H63 of C63, H34
  of C34, H22 of C22, {H66A,H66B} of C66
 At 1.5 times of:
  {H19A,H19B,H19C} of C19, H3 of O3, {H1A,H1B,H1C} of C1
2.a Ternary CH refined with riding coordinates:
 C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C67(H67A,H67B), C11(H11A,H11B), C66(H66A,H66B)
2.c Aromatic/amide H refined with riding coordinates:
 C43(H43), C55(H55), C38(H38), C39(H39), C54(H54), C49(H49), C47(H47),
 C50(H50), C64(H64), C37(H37), C56(H56), C23(H23), C32(H32), C65(H65), C8(H8),
 C4(H4), C41(H41), C24(H24), C6(H6), C14(H14), C15(H15), C5(H5), C46(H46),
 C48(H48), C31(H31), C61(H61), C58(H58), C12(H12), C40(H40), C21(H21), C16(H16),
  C35(H35), C27(H27), C52(H52), C53(H53), C62(H62), C25(H25), C33(H33),
 C63(H63), C34(H34), C22(H22)
2.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C1(H1A,H1B,H1C)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_fab_checksum              62081
_shelx_res_checksum              27937
_shelx_shelxl_version_number     2014/7