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_7045711
_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         'C46 H48 Dy2 N6 O20 Zn2'
_chemical_formula_sum            'C46 H48 Dy2 N6 O20 Zn2'
_chemical_formula_weight         1460.64
_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   geom
_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                90
_cell_angle_beta                 104.998(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1539(8)
_cell_length_b                   12.8094(7)
_cell_length_c                   18.1769(12)
_cell_measurement_reflns_used    8323
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.6910
_cell_measurement_theta_min      2.3390
_cell_volume                     2733.5(3)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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    -35.00  73.00   1.00   10.00    --  -17.00  72.00 150.00  108
  2  \w    -69.00  22.00   1.00   10.00    --  -17.00 -72.00  30.00   91
  3  \w    -69.00  22.00   1.00   10.00    --  -17.00 -72.00-150.00   91
  4  \w    -56.00   8.00   1.00   10.00    --  -17.00   0.00   0.00   64
  5  \w    -31.00 -14.00   1.00   10.00    --  -17.00  54.00   0.00   17
  6  \w   -107.00  30.00   1.00   10.00    --  -17.00 -18.00  60.00  137
  7  \w    -80.00 -29.00   1.00   10.00    --  -17.00 -72.00   0.00   51
;
_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      -0.0569793000
_diffrn_orient_matrix_UB_12      -0.0155937000
_diffrn_orient_matrix_UB_13      -0.0030496000
_diffrn_orient_matrix_UB_21      -0.0099177000
_diffrn_orient_matrix_UB_22      0.0472552000
_diffrn_orient_matrix_UB_23      0.0175481000
_diffrn_orient_matrix_UB_31      -0.0174214000
_diffrn_orient_matrix_UB_32      0.0242845000
_diffrn_orient_matrix_UB_33      -0.0362730000
_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     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7980
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.061
_diffrn_reflns_theta_max         25.061
_diffrn_reflns_theta_min         2.320
_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    3.647
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75174
_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    1.775
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by slow evaporation'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.195
_refine_diff_density_min         -2.539
_refine_diff_density_rms         0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         7980
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0953
_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^)+(0.1159P)^2^+99.0667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2490
_refine_ls_wR_factor_ref         0.2627
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6921
_reflns_number_total             7980
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9722\% 
 around [-0.45 0.00 0.89] (reciprocal) or [-0.67 0.00 0.74] (direct)
;
_cod_data_source_file            c8dt00538a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7045711--7045714.cif.'
_cod_database_code               7045711
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Zn Yb C22 H22 N4 O10'
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.839
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.560(3)
 0.440(3)
2. 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
3. Restrained distances
 C6A-C1A \\sim C1B-C6B \\sim C1A-C2 \\sim C3A-C2 \\sim C3A-C4A \\sim C3B-C4B
\\sim C5-C4B \\sim C6B-C5
 with sigma of 0.02
 C1B-C2 \\sim C1A-C2 \\sim C6A-C1A \\sim C1B-C6B \\sim C6A-C5 \\sim C6B-C5
\\sim C5-C4A \\sim C5-C4B \\sim C3A-
 C4A \\sim C3B-C4B \\sim C3B-C2 \\sim C3A-C2
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 C1A, C1B, C2, C3A, C3B, C4A, C4B, C5, C6A, C6B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C6B)=Sof(H6B)=Sof(C1B)=Sof(H1B)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(C3B)=
 Sof(H3BA)=Sof(H3BB)=1-FVAR(1)
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C6A)=Sof(H6A)=
 Sof(C1A)=Sof(H1A)=FVAR(1)
 Fixed Sof: H5AA(0.5) H5AB(0.5) H5BC(0.5) H5BD(0.5) H2AA(0.5) H2AB(0.5)
 H2BC(0.5) H2BD(0.5)
6.a Ternary CH refined with riding coordinates:
 C6A(H6A), C1A(H1A), C6B(H6B), C1B(H1B)
6.b Secondary CH2 refined with riding coordinates:
 C4A(H4AA,H4AB), C3A(H3AA,H3AB), C4B(H4BA,H4BB), C3B(H3BA,H3BB), C5(H5AA,H5AB),
  C5(H5BC,H5BD), C2(H2AA,H2AB), C2(H2BC,H2BD)
6.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C9(H9), C19(H19), C7(H7), C10(H10), C17(H17), C15(H15), C18(H18)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              94739
_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 KG0210052016
_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 2.544
_oxdiff_exptl_absorpt_empirical_full_min 0.482
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2