Dinucleating Schiff base ligand in Zn/4f coordination chemistry: synthetic challenges and catalytic activity evaluation.
Sampani, Stavroula I.; Aubert, Sidonie; Cattoen, Martin; Griffiths, Kieran; Abdul-Sada, Alaa; Akien, Geoffrey R.; Tizzard, Graham J.; Coles, Simon J.; Arseniyadis, Stellios; Kostakis, George E.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 4486–4493; doi:10.1039/c8dt00538a

data_7045713
_publ_section_title
;
 Dinucleating Schiff base ligand in Zn/4f coordination chemistry:
 synthetic challenges and catalytic activity evaluation.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4486
_journal_page_last               4493
_journal_paper_doi               10.1039/c8dt00538a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C24 H30 Cl Dy N4 O11 Zn'
_chemical_formula_sum            'C24 H30 Cl Dy N4 O11 Zn'
_chemical_formula_weight         813.84
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-27
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2018-01-30 deposited with the CCDC.
2018-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.819(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1433(4)
_cell_length_b                   8.2376(2)
_cell_length_c                   24.0684(5)
_cell_measurement_reflns_used    21814
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.3310
_cell_measurement_theta_min      3.2130
_cell_volume                     3193.56(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -38.00  27.00   0.50    3.00    --    0.00  60.00-150.00  130
  2  \w    -84.00 -54.00   0.50    3.00    --    0.00  60.00-150.00   60
  3  \w    -68.00  88.00   0.50    3.00    --    0.00  60.00 -90.00  312
  4  \w   -174.00-103.00   0.50   12.00    --  -90.00  20.00 -94.27  142
  5  \w   -164.00-119.00   0.50   12.00    --  -90.00  60.00-150.00   90
  6  \w    -89.00  -6.00   0.50   12.00    --  -90.00  60.00-150.00  166
  7  \w   -178.00  -2.00   0.50   12.00    --  -90.00   0.00  60.00  352
  8  \w    -26.00  -1.00   0.50   12.00    --  -90.00  60.00 -30.00   50
  9  \w   -178.00-115.00   0.50   12.00    --  -90.00  57.00-120.00  126
 10  \w    -30.00  -3.00   0.50   12.00    --  -90.00  29.00  30.00   54
 11  \w   -178.00-136.00   0.50   12.00    --  -90.00  60.00 120.00   84
 12  \w   -129.00 -91.00   0.50   12.00    --  -90.00  60.00 120.00   76
 13  \w    -40.00 -15.00   0.50   12.00    --  -90.00  60.00 120.00   50
 14  \w   -173.00 -27.00   0.50   12.00    --  -90.00  60.00 -90.00  292
 15  \w    -61.00 -30.00   0.50   12.00    --  -90.00  57.00 150.00   62
 16  \w   -170.00-134.00   0.50   12.00    --  -90.00  60.00   0.00   72
 17  \w   -161.00-123.00   0.50   12.00    --  -90.00  59.00   5.98   76
 18  \w    -84.00 -41.00   0.50   12.00    --  -90.00  59.00   5.98   86
 19  \w   -110.00 -85.00   0.50   12.00    --  -90.00  57.00-120.00   50
 20  \w   -118.00 -76.00   0.50   12.00    --  -90.00  29.00  30.00   84
 21  \w   -144.00 -77.00   0.50   12.00    --  -90.00  57.00 -60.00  134
 22  \w   -177.00-151.00   0.50   12.00    --  -90.00  60.00 -60.00   52
 23  \w   -143.00-118.00   0.50   12.00    --  -90.00  60.00 -60.00   50
 24  \w    -55.00 -28.00   0.50   12.00    --  -90.00  60.00 -60.00   54
 25  \w   -169.00 -84.00   0.50   12.00    --  -90.00  60.00-180.00  170
 26  \w    -76.00 -51.00   0.50   12.00    --  -90.00  60.00-180.00   50
 27  \w   -171.00-138.00   0.50   12.00    --  -90.00  43.00  90.00   66
 28  \w   -102.00 -62.00   0.50   12.00    --  -90.00  43.00  90.00   80
 29  \w    -44.00 -13.00   0.50   12.00    --  -90.00  43.00  90.00   62
 30  \w   -175.00-131.00   0.50   12.00    --  -90.00  14.00  90.00   88
 31  \w   -115.00 -88.00   0.50   12.00    --  -90.00  14.00  90.00   54
 32  \w   -173.00 -74.00   0.50   12.00    --  -90.00  57.00 150.00  198
 33  \w    -44.00 -19.00   0.50   12.00    --  -90.00  60.00   0.00   50
 34  \w   -134.00-103.00   0.50   12.00    --  -90.00  43.00-150.00   62
 35  \w    -53.00 -12.00   0.50   12.00    --  -90.00  43.00-150.00   82
 36  \w   -177.00-150.00   0.50   12.00    --  -90.00  57.00-180.00   54
 37  \w   -132.00-107.00   0.50   12.00    --  -90.00  57.00-180.00   50
 38  \w    -35.00 -10.00   0.50   12.00    --  -90.00  57.00-180.00   50
 39  \w   -170.00 -84.00   0.50   12.00    --  -90.00  60.00 -30.00  172
 40  \w    -40.00 -13.00   0.50   12.00    --  -90.00  20.00 -94.27   54
 41  \w    -54.00 -27.00   0.50   12.00    --  -90.00   0.00 -90.00   54
 42  \w   -168.00-102.00   0.50   12.00    --  -90.00  60.00  60.00  132
 43  \w   -110.00 -85.00   0.50   12.00    --  -90.00  59.00  44.92   50
 44  \w   -151.00  -1.00   0.50   12.00    --  -90.00  43.00 120.00  300
 45  \w   -136.00-109.00   0.50   12.00    --  -90.00  57.00   0.00   54
 46  \w   -155.00-128.00   0.50   12.00    --  -90.00  57.00  90.00   54
 47  \w   -103.00 -78.00   0.50   12.00    --  -90.00  57.00  90.00   50
 48  \w   -124.00 -97.00   0.50   12.00    --  -90.00  43.00 -30.00   54
 49  \w    -43.00 -18.00   0.50   12.00    --  -90.00  43.00 -30.00   50
 50  \w   -104.00 -75.00   0.50   12.00    --  -90.00  43.00   0.00   58
 51  \w    -40.00 -15.00   0.50   12.00    --  -90.00  43.00   0.00   50
 52  \w   -167.00-142.00   0.50   12.00    --  -90.00  59.00  44.92   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_diffrn_measurement_device_type
'Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0793248000
_diffrn_orient_matrix_UB_12      -0.0650390000
_diffrn_orient_matrix_UB_13      0.0244687000
_diffrn_orient_matrix_UB_21      0.0455927000
_diffrn_orient_matrix_UB_22      -0.1587580000
_diffrn_orient_matrix_UB_23      0.0166340000
_diffrn_orient_matrix_UB_31      0.0279970000
_diffrn_orient_matrix_UB_32      0.0743398000
_diffrn_orient_matrix_UB_33      0.0569067000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_reflns_av_R_equivalents  0.0967
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            61655
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.056
_diffrn_reflns_theta_min         3.200
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    14.585
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       block
_exptl_crystal_F_000             1612
_exptl_crystal_recrystallization_method
'The material was recrystallised from ethanol by slow evaporation'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.096
_refine_diff_density_min         -1.716
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         6046
_refine_ls_number_restraints     630
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0996P)^2^+1.3153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4957
_reflns_number_total             6046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00538a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7045711--7045714.cif.'
_cod_database_code               7045713
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C92 H108 Cl4 Dy4 N12 O44 Zn4 '
_chemical_oxdiff_usercomment     SS419
_shelx_estimated_absorpt_t_max   0.669
_shelx_estimated_absorpt_t_min   0.323
_diffrn_oxdiff_ac3_digest_frames
;
01f9e576944edae6512df99d104723c5230500274eb
;
_diffrn_oxdiff_ac3_digest_hkl
;
01bd4d5c64dd6d7b408b38c65f77f4d2f63024
;
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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, All O(H) groups
2. Restrained distances
 O5-H5
 0.85 with sigma of 0.01
 C23-H5
 1.925921 with sigma of 0.02
 Dy1-H5
 2.817452 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=
 Sof(H4BC)=Sof(H4BD)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C6B)=Sof(H6B)=1-FVAR(1)
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=
 Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=Sof(H6A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1A(H1A), C1B(H1B), C6A(H6A), C6B(H6B)
5.b Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C2B(H2BA,H2BB), C3A(H3AA,H3AB), C3B(H3BA,H3BB), C4(H4AA,H4AB),
  C4(H4BC,H4BD), C5A(H5AA,H5AB), C5B(H5BA,H5BB), C23(H23A,H23B)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C10(H10), C11(H11), C15(H15), C17(H17), C18(H18), C19(H19)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              53502
_shelx_fab_checksum              79716
_olex2_date_sample_data_collection 2017-07-24
_olex2_date_sample_submission    2017-06-29
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id SS419
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.136
_oxdiff_exptl_absorpt_empirical_full_min 0.476