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_1546878
_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         'C48 H58 Er2 N4 Ni2 O22'
_chemical_formula_sum            'C48 H58 Er2 N4 Ni2 O22'
_chemical_formula_weight         1494.88
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-31
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_audit_update_record
;
2017-08-14 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.402(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8413(3)
_cell_length_b                   14.1659(5)
_cell_length_c                   17.3158(5)
_cell_measurement_reflns_used    8133
_cell_measurement_temperature    128.55(10)
_cell_measurement_theta_max      28.9370
_cell_measurement_theta_min      3.0960
_cell_volume                     3147.12(16)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies,Version 1.171.36.28'
_computing_data_collection
'CrysAlisPro, Agilent Technologies,Version 1.171.36.28'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies,Version 1.171.36.28'
_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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      128.55(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
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_diffrn_reflns_limit_l_min       -20
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_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.876
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.300
_exptl_absorpt_correction_T_max  0.660
_exptl_absorpt_correction_T_min  0.592
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
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_exptl_crystal_size_max          0.21
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_refine_diff_density_max         0.939
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5539
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+1.4598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0667
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5080
_reflns_number_total             5549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02351k2.cif
_cod_data_source_block           p131231h_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               1546878
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H10 of C10, H6 of C6, H5 of C5, {H22a,H22b} of C22, H15 of C15, H12 of C12,
  H14 of C14, {H9a,H9b} of C9, {H11a,H11b} of C11, H8 of C8, H16 of C16, H4 of
  C4
 At 1.5 times of:
  {H23a,H23b,H23c} of C23, {H21a,H21b,H21c} of C21, H11 of O11, {H19a,H19b,
  H19c} of C19, {H1a,H1b,H1c} of C1, H3 of O3
2. Restrained distances
 O11-H11
 0.85 with sigma of 0.01
 C22-H11
 1.907709 with sigma of 0.02
 Ni1-H11
 2.716305 with sigma of 0.02
3. Rigid bond restraints
 C24, O7
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 C24, O8
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 O7, C24
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 C24, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C24 ~ O6 ~ O8 ~ O7: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
5.a Ternary CH refined with riding coordinates:
 C10(H10)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C22(H22a,H22b), C9(H9a,H9b)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C16(H16), C8(H8), C6(H6), C5(H5), C15(H15), C12(H12), C14(H14)
5.d Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C19(H19a,H19b,H19c), C21(H21a,H21b,H21c), C23(H23a,H23b,H23c)
5.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_fab_checksum              31925
_shelx_res_checksum              73292
_shelx_shelxl_version_number     2014/7