Tetranuclear Zn/4f coordination clusters as highly efficient catalysts for Friedel-Crafts alkylation
Griffiths, Kieran; Kumar, Prashant; Akien, Geoffrey R.; Chilton, Nicholas F.; Abdul-Sada, Alaa; Tizzard, Graham J.; Coles, Simon J.; Kostakis, George E.; Chemical Communications 52 (2016) 7866–7869; doi:10.1039/c6cc03608b

data_7119381
_publ_section_title
;
 Tetranuclear Zn/4f coordination clusters as highly efficient catalysts
 for Friedel-Crafts alkylation
;
_journal_issue                   50
_journal_name_full               'Chemical Communications'
_journal_page_first              7866
_journal_page_last               7869
_journal_paper_doi               10.1039/c6cc03608b
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C62 H58 N8 O20 Y2 Zn2'
_chemical_formula_sum            'C62 H58 N8 O20 Y2 Zn2'
_chemical_formula_weight         1543.72
_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     direct
_audit_creation_date             2015-05-17
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Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
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_audit_update_record
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2016-02-09 deposited with the CCDC.
2016-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.068(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.7448(6)
_cell_length_b                   14.3133(7)
_cell_length_c                   16.9268(7)
_cell_measurement_reflns_used    2990
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1900
_cell_measurement_theta_min      4.2300
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.849
_diffrn_measured_fraction_theta_max 0.700
_diffrn_measurement_details
;
  1 omega  -39.00   55.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.1295   19.0000 -150.0000 94

  2 omega   -3.00   52.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.1295   38.0000  -60.0000 55
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_11      0.0304666000
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_diffrn_orient_matrix_UB_13      0.0358032000
_diffrn_orient_matrix_UB_21      -0.0121706000
_diffrn_orient_matrix_UB_22      0.0481186000
_diffrn_orient_matrix_UB_23      0.0004221000
_diffrn_orient_matrix_UB_31      -0.0400769000
_diffrn_orient_matrix_UB_32      -0.0103175000
_diffrn_orient_matrix_UB_33      0.0221422000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.849
_diffrn_reflns_Laue_measured_fraction_max 0.700
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
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_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10546
_diffrn_reflns_point_group_measured_fraction_full 0.849
_diffrn_reflns_point_group_measured_fraction_max 0.700
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.323
_diffrn_reflns_theta_min         3.385
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.525
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_F_000             1568
_refine_diff_density_max         2.248
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         6364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0791
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+6.4200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1627
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4932
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc03608b2.cif
_cod_data_source_block           1Y
_cod_database_code               7119381
_chemical_oxdiff_formula         Y2ZN2C80H100N12O24
_reflns_odcompleteness_completeness 84.08
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00O(H00O), C00Q(H00Q), C00S(H00S), C00U(H00U), C00V(H00V),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C011(H011), C012(H012), C013(H013),
 C014(H014), C015(H015), C016(H016), C017(H017), C018(H018)
2.b Idealised Me refined as rotating group:
 C00W(H00A,H00B,H00C), C010(H01A,H01B,H01C), C01A(H01D,H01E,H01F), C01B(H01G,
 H01H,H01I)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'