Four Salamo-type 3d-4f hetero-bimetallic [ZnIILnIII] complexes: Syntheses, Crystal Structures, Luminescent and Magnetic Properties
Zheng, Shan shan; Dong, WK; Zhang, Yang; Chen, Le; Ding, Yujie; New J. Chem. 41 (2017) 4966–4973; doi:10.1039/C6NJ04090J

data_7056169
_publ_section_title
;
 Four Salamo-type 3d-4f hetero-bimetallic [ZnIILnIII] complexes:
 Syntheses, Crystal Structures, Luminescent and Magnetic Properties
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              4966
_journal_page_last               4973
_journal_paper_doi               10.1039/C6NJ04090J
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C22 H25 Eu N4 O14 Zn'
_chemical_formula_sum            'C22 H25 Eu N4 O14 Zn'
_chemical_formula_weight         786.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-12-23 deposited with the CCDC.
2017-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.442(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1508(7)
_cell_length_b                   13.2769(5)
_cell_length_c                   16.3725(9)
_cell_measurement_reflns_used    1754
_cell_measurement_temperature    298.84(10)
_cell_measurement_theta_max      25.3440
_cell_measurement_theta_min      3.4950
_cell_volume                     2768.3(2)
_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  'XL (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      298.84(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega    0.00   93.45   1.0500    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   57.0000  -90.0000 89

  2 omega   36.00   90.60   1.0500    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   57.0000 -180.0000 52

  3 omega   -4.00   21.20   1.0500    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5055  -99.0000 -150.0000 24

  4 omega   34.00  103.30   1.0500    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867 -178.0000 -150.0000 66
;
_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      0.0087638000
_diffrn_orient_matrix_UB_12      -0.0527438000
_diffrn_orient_matrix_UB_13      0.0029401000
_diffrn_orient_matrix_UB_21      -0.0536357000
_diffrn_orient_matrix_UB_22      -0.0085022000
_diffrn_orient_matrix_UB_23      -0.0202003000
_diffrn_orient_matrix_UB_31      0.0122636000
_diffrn_orient_matrix_UB_32      0.0003874000
_diffrn_orient_matrix_UB_33      -0.0397892000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.1086
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11088
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.33
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.188
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98658
_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_density_diffrn    1.888
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.305
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5445
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                3579
_reflns_number_total             5445
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6nj04090j2.cif
_cod_data_source_block           d956
_cod_database_code               7056169
_reflns_odcompleteness_completeness 99.73
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H4-H2BC
 2.2 with sigma of 0.02
3. Others
 Fixed Sof: C1(0.65) H1A(0.65) H1B(0.65) H1C(0.65) H2AA(0.65) H2AB(0.65)
 H2BC(0.35) H2BD(0.35) C0AA(0.35) H0AA(0.35) H0AB(0.35) H0AC(0.35)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2AA,H2AB), C2(H2BC,H2BD), C10(H10A,H10B), C11(H11A,H11B), C19(H19A,H19B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C9(H9), C12(H12), C16(H16), C17(H17), C18(H18)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C0AA(H0AA,H0AB,H0AC)
;
_olex2_submission_special_instructions 'No special instructions were received'