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_7045712
_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         'C31 H35 N4 O14 Y Zn, C H4 O'
_chemical_formula_sum            'C32 H39 N4 O15 Y Zn'
_chemical_formula_weight         873.95
_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             2017-11-21
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2018-01-30 deposited with the CCDC.
2018-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                99.823(9)
_cell_angle_beta                 98.676(10)
_cell_angle_gamma                95.680(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0130(15)
_cell_length_b                   12.9690(15)
_cell_length_c                   13.1459(14)
_cell_measurement_reflns_used    1690
_cell_measurement_temperature    173
_cell_measurement_theta_max      62.7990
_cell_measurement_theta_min      4.4890
_cell_volume                     1813.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds): 
1 \w -43.00 98.00 1.00 1.50 -- 31.83 -19.00 60.00 141 
2 \w 43.00 74.00 1.00 1.50 -- 31.83 -99.00 0.00 31 
3 \w 25.00 89.00 1.00 4.00 -- 94.50-111.00 30.00 64 
4 \w 77.00 102.00 1.00 4.00 -- 94.50 -93.00 65.68 25 
5 \w 81.00 127.00 1.00 4.00 -- 94.50 -77.00 30.00 46 
6 \w 107.00 138.00 1.00 4.00 -- 94.50 -25.00 90.00 31 
7 \w 132.00 157.00 1.00 4.00 -- 94.50 25.00 90.00 25 
8 \w 138.00 164.00 1.00 4.00 -- 94.50 50.00 30.00 26 
9 \w 121.00 156.00 1.00 4.00 -- 94.50 77.00 120.00 35 
10 \w 98.00 139.00 1.00 4.00 -- 94.50 25.00 30.00 41 
11 \w 87.00 124.00 1.00 4.00 -- 94.50 -38.00 120.00 37 
12 \w 72.00 134.00 1.00 4.00 -- 94.50 -92.00 120.00 62 
13 \w 80.00 105.00 1.00 4.00 -- 94.50 -92.00 -30.00 25 
14 \w 83.00 128.00 1.00 4.00 -- 94.50 -92.00 -60.00 45 
15 \w 85.00 110.00 1.00 4.00 -- 94.50 -92.00-150.00 25 
16 \w 49.00 76.00 1.00 4.00 -- 94.50 -77.00-150.00 27 
17 \w 22.00 90.00 1.00 4.00 -- 94.50-111.00 -60.00 68 
18 \w 37.00 115.00 1.00 4.00 -- 94.50 -50.00 0.00 78 
19 \w 67.00 168.00 1.00 4.00 -- 94.50 38.00 120.00 101 
20 \w 81.00 134.00 1.00 4.00 -- 94.50 50.00 30.00 53 
21 \w 76.00 122.00 1.00 4.00 -- 94.50 64.00 -90.00 46 
22 \w 117.00 145.00 1.00 4.00 -- 94.50 50.00-120.00 28 
23 \w 131.00 158.00 1.00 4.00 -- 94.50 64.00-150.00 27 
24 \w 71.00 157.00 1.00 4.00 -- 94.50 25.00-180.00 86 
25 \w 69.00 104.00 1.00 4.00 -- 94.50 64.00-150.00 35 
26 \w 39.00 70.00 1.00 1.50 -- 31.83 178.00 -30.00 31 
27 \w 49.00 76.00 1.00 4.00 -- 94.50 -25.00 90.00 27 
28 \w 45.00 82.00 1.00 4.00 -- 94.50 -64.00 90.00 37 
29 \w 49.00 74.00 1.00 4.00 -- 94.50-111.00 60.00 25 
30 \w 44.00 88.00 1.00 4.00 -- 94.50 -64.00 120.00 44 
31 \w 30.00 57.00 1.00 4.00 -- 94.50-111.00 0.00 27 
32 \w 22.00 78.00 1.00 4.00 -- 94.50 -92.00 -30.00 56 
33 \w 21.00 73.00 1.00 4.00 -- 94.50-111.00 -30.00 52 
34 \w 21.00 86.00 1.00 4.00 -- 94.50-111.00 90.00 65 
35 \w -11.00 38.00 1.00 1.50 -- 31.83 -99.00 0.00 49 
36 \w -88.00 -57.00 1.00 1.50 -- -31.83-178.00-180.00 31 
37 \w -100.00 -59.00 1.00 1.50 -- -31.83 -38.00 30.00 41 

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1388662000
_diffrn_orient_matrix_UB_12      -0.0334319000
_diffrn_orient_matrix_UB_13      -0.0029696000
_diffrn_orient_matrix_UB_21      -0.0278356000
_diffrn_orient_matrix_UB_22      0.0146255000
_diffrn_orient_matrix_UB_23      -0.1147076000
_diffrn_orient_matrix_UB_31      0.0173866000
_diffrn_orient_matrix_UB_32      -0.1159585000
_diffrn_orient_matrix_UB_33      -0.0375038000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_unetI/netI     0.0819
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12577
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        63.150
_diffrn_reflns_theta_max         63.150
_diffrn_reflns_theta_min         4.429
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.610
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (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    1.600
_exptl_crystal_description       plate
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.136
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         5627
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0653
_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^)+(0.0880P)^2^+3.1130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1957
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3832
_reflns_number_total             5627
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00538a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7045711--7045714.cif.'
_cod_database_code               7045712
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Zn Y C30 H30 N2 O10'
_reflns_odcompleteness_completeness 84.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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
 C25-H13
 1.867934 with sigma of 0.02
 Y1-H13
 2.869091 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C9(H9), C14(H14)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C15(H15), C17(H17), C18(H18), C19(H19),
 C27(H27), C29(H29), C30(H30), C31(H31)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C34(H34A,H34B,
 H34C), C26(H26A,H26B,H26C)
3.e Idealised tetrahedral OH refined as rotating group:
 O14(H14A)
;
_olex2_date_sample_data_collection 2017-11-17
_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 1.896
_oxdiff_exptl_absorpt_empirical_full_min 0.644