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_7119382
_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 Eu2 N8 O20 Zn2'
_chemical_formula_sum            'C62 H58 Eu2 N8 O20 Zn2'
_chemical_formula_weight         1669.82
_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             2016-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-02-09 deposited with the CCDC.
2016-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.498(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8125(4)
_cell_length_b                   14.3087(5)
_cell_length_c                   16.9783(5)
_cell_measurement_reflns_used    7576
_cell_measurement_temperature    173
_cell_measurement_theta_max      61.0100
_cell_measurement_theta_min      4.0170
_cell_volume                     3340.14(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_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     33.00 100.00   1.00    1.00    --   36.88  57.00   0.00   67
  2  \w     79.00 156.00   1.00    4.50    --   86.50  30.00 -90.00   77
  3  \w     97.00 146.00   1.00    4.50    --   86.50 111.00-180.00   49
  4  \w     66.00 112.00   1.00    4.50    --   86.50  77.00-180.00   46
  5  \w     55.00  82.00   1.00    4.50    --   86.50 -33.00  -6.29   27
  6  \w     39.00  64.00   1.00    4.50    --   86.50 -30.00  30.00   25
  7  \w     55.00 133.00   1.00    4.50    --   86.50  18.00  98.39   78
  8  \w    105.00 130.00   1.00    4.50    --   86.50  77.00  30.00   25
  9  \w     98.00 124.00   1.00    4.50    --   86.50 111.00 150.00   26
 10  \w     20.00  83.00   1.00    4.50    --   86.50 -45.00  90.00   63
 11  \w     78.00 110.00   1.00    4.50    --   86.50 -93.00 121.66   32
 12  \w     63.00  90.00   1.00    4.50    --   86.50-111.00  90.00   27
 13  \w     63.00  89.00   1.00    4.50    --   86.50-111.00 150.00   26
 14  \w     66.00  98.00   1.00    4.50    --   86.50-129.00 165.00   32
 15  \w     31.00  57.00   1.00    4.50    --   86.50 -95.00  60.00   26
 16  \w     67.00 119.00   1.00    4.50    --   86.50 -92.00  -1.96   52
 17  \w     33.00  59.00   1.00    4.50    --   86.50-111.00 -60.00   26
 18  \w     21.00  93.00   1.00    4.50    --   86.50 -61.00 -90.00   72
 19  \w     55.00 106.00   1.00    4.50    --   86.50 -77.00-180.00   51
 20  \w    -22.00  76.00   1.00    1.00    --   36.88 -99.00 -90.00   98
 21  \w     27.00  53.00   1.00    4.50    --   86.50-129.00 165.00   26
 22  \w   -109.00 -84.00   1.00    1.00    --  -36.88-178.00-120.00   25
;
_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      -0.0182953000
_diffrn_orient_matrix_UB_12      -0.0391325000
_diffrn_orient_matrix_UB_13      -0.0847155000
_diffrn_orient_matrix_UB_21      -0.0001440000
_diffrn_orient_matrix_UB_22      0.1000849000
_diffrn_orient_matrix_UB_23      -0.0333970000
_diffrn_orient_matrix_UB_31      0.1105181000
_diffrn_orient_matrix_UB_32      -0.0063941000
_diffrn_orient_matrix_UB_33      -0.0050798000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17052
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         61.143
_diffrn_reflns_theta_min         4.460
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.709
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.628
_refine_diff_density_min         -1.019
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         5096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0704P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4560
_reflns_number_total             5096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc03608b2.cif
_cod_data_source_block           1Eu
_cod_original_cell_volume        3340.12(18)
_cod_database_code               7119382
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         Zn2Eu2C60H100N16O16
_reflns_odcompleteness_completeness 85.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C00J(H00J), C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00T(H00T),
 C00U(H00U), C00V(H00V), C00Y(H00Y), C00Z(H00Z), C011(H011), C012(H012),
 C013(H013), C014(H014), C015(H015), C016(H016), C017(H017)
2.b Idealised Me refined as rotating group:
 C018(H01A,H01B,H01C), C019(H01D,H01E,H01F), C01A(H01G,H01H,H01I), C01B(H01J,
 H01K,H01L)
;
_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 1.661
_oxdiff_exptl_absorpt_empirical_full_min 0.688