Nine self-assembled nickel(ii)–lanthanide(iii) heterometallic complexes constructed from a Salamo-type bisoxime and bearing a N- or O-donor auxiliary ligand: syntheses, structures and magnetic properties
Dong, Wen-Kui; Ma, Jian-Chun; Zhu, Li-Chun; Zhang, Yang; New J. Chem. 40 (2016) 6998–; doi:10.1039/C6NJ00855K

data_7055622
_publ_section_title
;
 Nine self-assembled nickel(ii)--lanthanide(iii) heterometallic complexes
 constructed from a Salamo-type bisoxime and bearing a N- or O-donor
 auxiliary ligand: syntheses, structures and magnetic properties
;
_journal_issue                   8
_journal_name_full               'New J. Chem.'
_journal_page_first              6998
_journal_paper_doi               10.1039/C6NJ00855K
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C52 H62 La2 N10 Ni2 O32'
_chemical_formula_sum            'C52 H62 La2 N10 Ni2 O32'
_chemical_formula_weight         1734.35
_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     iterative
_audit_creation_date             2015-10-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-11-01 deposited with the CCDC.
2016-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.2166(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.3389(3)
_cell_length_b                   13.0476(4)
_cell_length_c                   17.2529(4)
_cell_measurement_reflns_used    4817
_cell_measurement_temperature    293.42(10)
_cell_measurement_theta_max      27.4780
_cell_measurement_theta_min      3.5410
_cell_volume                     3425.57(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.42(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -16.00   16.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000  120.0000 32

  2 omega  -26.00   18.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000  120.0000 44

  3 omega   14.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   38.0000  -90.0000 79

  4 omega   42.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  178.0000  150.0000 53

  5 omega  -45.00  -13.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000 -180.0000 32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0152966000
_diffrn_orient_matrix_UB_12      0.0009268000
_diffrn_orient_matrix_UB_13      -0.0405257000
_diffrn_orient_matrix_UB_21      -0.0112060000
_diffrn_orient_matrix_UB_22      -0.0526268000
_diffrn_orient_matrix_UB_23      0.0014652000
_diffrn_orient_matrix_UB_31      -0.0426260000
_diffrn_orient_matrix_UB_32      0.0134756000
_diffrn_orient_matrix_UB_33      0.0084611000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14180
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.352
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.857
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       block
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6714
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0232P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0904
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5138
_reflns_number_total             6714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj00855k1.cif
_cod_data_source_block           d655_2
_cod_depositor_comments
'Adding full bibliography for 7055617--7055625.cif.'
_cod_original_cell_volume        3425.58(14)
_cod_database_code               7055622
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2. Restrained distances
 O13-H13
 0.85 with sigma of 0.01
 C23-H13
 1.898803 with sigma of 0.02
 Ni1-H13
 2.671219 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C9(H9A,H9B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C14(H14), C21(H21), C8(H8), C7(H7), C22(H22), C26(H26), C11(H11),
 C5(H5), C13(H13A), C15(H15)
3.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C18(H18A,H18B,H18C), C1(H1A,H1B,H1C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C)
;
_olex2_date_sample_data_collection 2015-04-08
_olex2_submission_special_instructions 'No special instructions were received'