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_7119380
_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 Dy2 N8 O20 Zn2'
_chemical_formula_sum            'C62 H58 Dy2 N8 O20 Zn2'
_chemical_formula_weight         1690.90
_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
_audit_creation_date             2015-04-23
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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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                 95.2801(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.75033(18)
_cell_length_b                   14.3147(2)
_cell_length_c                   16.9418(2)
_cell_measurement_reflns_used    6986
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.1670
_cell_measurement_theta_min      3.6210
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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)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
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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)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_details
;
  1 omega  -84.00   13.00   1.0000   41.4950
omega____ theta____ kappa____ phi______ frames
    -      -15.9733  -19.0000  -90.0000 97

  2 omega  -87.00   10.00   1.0000   41.4950
omega____ theta____ kappa____ phi______ frames
    -      -15.9733  -19.0000    0.0000 97
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_11      0.0254056000
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_diffrn_orient_matrix_UB_13      0.0184206000
_diffrn_orient_matrix_UB_21      -0.0428540000
_diffrn_orient_matrix_UB_22      0.0134696000
_diffrn_orient_matrix_UB_23      0.0173635000
_diffrn_orient_matrix_UB_31      0.0141700000
_diffrn_orient_matrix_UB_32      -0.0281236000
_diffrn_orient_matrix_UB_33      0.0335598000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.980
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_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14238
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         3.383
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.016
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86544
_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    1.691
_exptl_crystal_F_000             1676
_refine_diff_density_max         2.514
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         7145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0462
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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^)+(0.0453P)^2^+6.2412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6118
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc03608b2.cif
_cod_data_source_block           1Dy
_cod_original_cell_volume        3320.55(8)
_cod_database_code               7119380
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         Zn2Dy2C80H100N14O12
_reflns_odcompleteness_completeness 98.52
_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:
 C00K(H00K), C00N(H00N), C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T),
 C00V(H00V), C00X(H00X), C00Z(H00Z), C010(H010), C011(H011), C013(H013),
 C014(H014), C015(H015), C016(H016), C017(H017), C018(H018)
2.b Idealised Me refined as rotating group:
 C00Y(H00A,H00B,H00C), C019(H01A,H01B,H01C), C01A(H01D,H01E,H01F), C01B(H01G,
 H01H,H01I)
;
_shelx_res_checksum              11635
_olex2_submission_special_instructions 'No special instructions were received'