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_7045714
_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 N4 O11 Y Zn'
_chemical_formula_sum            'C24 H30 Cl N4 O11 Y Zn'
_chemical_formula_weight         740.25
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-01
_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                67.998(4)
_cell_angle_beta                 83.196(3)
_cell_angle_gamma                80.804(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2025(3)
_cell_length_b                   14.3533(5)
_cell_length_c                   14.4172(6)
_cell_measurement_reflns_used    9214
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.7640
_cell_measurement_theta_min      2.5090
_cell_volume                     1550.35(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.970
_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   -107.00  73.00   1.00    5.00    --  -17.00   0.00 -60.00  180
  2  \w    -69.00  22.00   1.00    5.00    --  -17.00 -72.00 -90.00   91
  3  \w    -75.00  22.00   1.00    5.00    --  -17.00 -72.00 120.00   97
  4  \w    -27.00  68.00   1.00    5.00    --  -17.00  72.00  30.00   95
  5  \w    -49.00 -32.00   1.00    5.00    --  -17.00 -72.00  90.00   17
  6  \w   -107.00 -31.00   1.00    5.00    --  -17.00   0.00  30.00   76
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0097895000
_diffrn_orient_matrix_UB_12      -0.0097090000
_diffrn_orient_matrix_UB_13      0.0522093000
_diffrn_orient_matrix_UB_21      0.0415843000
_diffrn_orient_matrix_UB_22      -0.0496807000
_diffrn_orient_matrix_UB_23      0.0097497000
_diffrn_orient_matrix_UB_31      0.0766824000
_diffrn_orient_matrix_UB_32      0.0179917000
_diffrn_orient_matrix_UB_33      -0.0025190000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18089
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.534
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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    1.586
_exptl_crystal_description       plate
_exptl_crystal_F_000             752
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by slow evaporation'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6903
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0671P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1205
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5271
_reflns_number_total             6903
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00538a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7045711--7045714.cif.'
_cod_database_code               7045714
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         '(Zn2 Y2 (C22 H24 N2 O2)2 (N O3)4 )2 (N O3)'
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.680
_reflns_odcompleteness_completeness 96.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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
 1.91398 with sigma of 0.02
 Y1-H5
 2.80439 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C4A \\sim C3B \\sim C3A \\sim C4B \\sim C1B \\sim C1A \\sim C6B \\sim C6A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C6A, C6B, C1A, C1B, C4B, C4A, C3A, C3B, C2, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H5bc)=Sof(H5bd)=Sof(H2bc)=Sof(H2bd)=Sof(C1B)=Sof(H1B)=Sof(C6A)=Sof(H6A)=
 Sof(C3B)=Sof(H3Ba)=Sof(H3Bb)=Sof(C4B)=Sof(H4Ba)=Sof(H4Bb)=1-FVAR(1)
 Sof(H5aa)=Sof(H5ab)=Sof(H2aa)=Sof(H2ab)=Sof(C6B)=Sof(H6B)=Sof(C1A)=Sof(H1A)=
 Sof(C3A)=Sof(H3Aa)=Sof(H3Ab)=Sof(C4A)=Sof(H4Aa)=Sof(H4Ab)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C6B(H6B), C1A(H1A), C1B(H1B), C6A(H6A)
6.b Secondary CH2 refined with riding coordinates:
 C5(H5aa,H5ab), C5(H5bc,H5bd), C2(H2aa,H2ab), C2(H2bc,H2bd), C23(H23a,H23b),
 C3A(H3Aa,H3Ab), C4A(H4Aa,H4Ab), C3B(H3Ba,H3Bb), C4B(H4Ba,H4Bb)
6.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C19(H19), C7(H7), C9(H9), C15(H15), C17(H17), C18(H18)
6.d Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C22(H22a,H22b,H22c), C24(H24a,H24b,H24c)
;
_shelx_res_checksum              72759
_shelx_fab_checksum              20554
_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 Zn-Y_CC
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.626
_oxdiff_exptl_absorpt_empirical_full_min 0.366