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_1546874
_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         'C66 H60 Cl4 Gd N2 Ni O11'
_chemical_formula_sum            'C66 H60 Cl4 Gd N2 Ni O11'
_chemical_formula_weight         1414.90
_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
_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                82.268(15)
_cell_angle_beta                 83.837(11)
_cell_angle_gamma                77.065(11)
_cell_formula_units_Z            2
_cell_length_a                   11.2556(16)
_cell_length_b                   12.667(2)
_cell_length_c                   23.339(4)
_cell_measurement_reflns_used    10905
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3203.3(9)
_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
;
_diffrn_ambient_temperature      113
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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: 44.8843
              2theta: -15.1083
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: 90.0000
                 XTD: 44.8843
              2theta: -15.1083
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: 180.0000
                 XTD: 44.8843
              2theta: -15.1083
;
_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      0.036249
_diffrn_orient_matrix_UB_12      0.069716
_diffrn_orient_matrix_UB_13      0.046785
_diffrn_orient_matrix_UB_21      -0.079732
_diffrn_orient_matrix_UB_22      0.016777
_diffrn_orient_matrix_UB_23      0.002904
_diffrn_orient_matrix_UB_31      0.000520
_diffrn_orient_matrix_UB_32      -0.027392
_diffrn_orient_matrix_UB_33      0.033633
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            41041
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.575
_diffrn_reflns_theta_min         3.039
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.546
_exptl_absorpt_correction_T_max  0.757
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1436
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.798
_refine_diff_density_min         -1.481
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         14485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0332P)^2^+6.8699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13455
_reflns_number_total             14485
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02351k2.cif
_cod_data_source_block           m20160305a_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               1546874
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H10A,H10B} of C10, {H66A,H66B} of C66, H31 of C31, H47 of C47, H41 of C41,
  H40 of C40, {H22A,H22B} of C22, H25 of C25, H3A of C3, H35 of C35, H64 of C64,
   H9 of C9, {H37A,H37B} of C37, {H12A,H12B} of C12, H46 of C46, H29 of C29,
  H57 of C57, H11 of C11, {H52A,H52B} of C52, H43 of C43, H62 of C62, H63 of
  C63, H42 of C42, H58 of C58, H56 of C56, H59 of C59, H49 of C49, H61 of C61,
  H44 of C44, H33 of C33, H28 of C28, H50 of C50, H13 of C13, H17 of C17, H65
  of C65, H32 of C32, H15 of C15, H5 of C5, H4 of C4, H16 of C16, H55 of C55,
  H27 of C27, H48 of C48, H26 of C26, H34 of C34, {H67A,H67B} of C67
 At 1.5 times of:
  H3 of O3, {H1A,H1B,H1C} of C1, {H20A,H20B,H20C} of C20
2.a Ternary CH refined with riding coordinates:
 C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C12(H12A,H12B), C37(H37A,H37B), C22(H22A,H22B), C66(H66A,
 H66B), C10(H10A,H10B), C67(H67A,H67B)
2.c Aromatic/amide H refined with riding coordinates:
 C43(H43), C62(H62), C63(H63), C42(H42), C58(H58), C56(H56), C59(H59),
 C49(H49), C61(H61), C44(H44), C33(H33), C28(H28), C50(H50), C13(H13), C17(H17),
  C65(H65), C32(H32), C15(H15), C5(H5), C4(H4), C16(H16), C55(H55), C57(H57),
 C29(H29), C46(H46), C9(H9), C64(H64), C35(H35), C3(H3A), C25(H25), C40(H40),
 C41(H41), C47(H47), C31(H31), C27(H27), C48(H48), C26(H26), C34(H34)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C20(H20A,H20B,H20C)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_fab_checksum              78853
_shelx_res_checksum              73655
_shelx_shelxl_version_number     2014/7