Tetranuclear Zn2Ln2 Coordination Clusters as catalysts in Petasis Borono-Mannich Multicomponent Reaction
Kumar, Prashant; Griffiths, Kieran; Lymperopoulou, Smaragda; Kostakis, George E.; RSC Adv.  (2016) –; doi:10.1039/C6RA17209A

data_7226253
_publ_section_title
;
 Tetranuclear Zn2Ln2 Coordination Clusters as catalysts in Petasis
 Borono-Mannich Multicomponent Reaction
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA17209A
_journal_year                    2016
_chemical_formula_moiety         'C17 H19 N O2'
_chemical_formula_sum            'C17 H19 N O2'
_chemical_formula_weight         269.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_symmetry_space_group_name_Hall  'I -2ya'
_symmetry_space_group_name_H-M   'I 1 a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-18 deposited with the CCDC.
2016-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.109(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4472(5)
_cell_length_b                   9.3180(4)
_cell_length_c                   11.5805(4)
_cell_measurement_reflns_used    2792
_cell_measurement_temperature    173
_cell_measurement_theta_max      70.8380
_cell_measurement_theta_min      5.7590
_cell_volume                     1451.05(10)
_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    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w   -109.00 -83.00   1.00    7.50    --  -36.88-178.00  60.00   26
  2  \w    -78.00 -18.00   1.00    7.50    --  -36.88 -38.00-180.00   60
  3  \w    -52.00  26.00   1.00    7.50    --  -36.88  57.00 -30.00   78
  4  \w   -103.00 -71.00   1.00    7.50    --  -36.88 147.00-168.00   32
  5  \w     39.00 106.00   1.00    7.50    --   36.88 178.00 120.00   67
  6  \w     12.00 102.00   1.00    7.50    --   36.88  77.00  90.00   90
  7  \w     37.00 102.00   1.00    7.50    --   36.88  57.00-180.00   65
  8  \w     97.00 123.00   1.00   17.50    --  107.00  45.00  90.00   26
  9  \w     96.00 178.00   1.00   17.50    --  107.00  15.00-150.00   82
 10  \w     59.00 122.00   1.00   17.50    --  107.00 -91.00  26.48   63
 11  \w     39.00 114.00   1.00   17.50    --  107.00 -45.00 -30.00   75
 12  \w     40.00 122.00   1.00   17.50    --  107.00 -45.00 150.00   82
 13  \w    100.00 171.00   1.00   17.50    --  107.00  77.00 120.00   71
 14  \w     38.00  72.00   1.00   17.50    --  107.00 -95.00 -30.00   34
 15  \w     38.00  80.00   1.00   17.50    --  107.00 -95.00 -60.00   42
 16  \w     90.00 144.00   1.00   17.50    --  107.00  45.00 -90.00   54
 17  \w    138.00 175.00   1.00   17.50    --  107.00  45.00  90.00   37
 18  \w     40.00 117.00   1.00   17.50    --  107.00 -45.00  60.00   77
 19  \w     41.00 114.00   1.00   17.50    --  107.00 -92.00-177.46   73
 20  \w     58.00  97.00   1.00   17.50    --  107.00 -91.00 119.39   39
 21  \w     92.00 128.00   1.00   17.50    --  107.00 -91.00-104.98   36
;
_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      -0.1110577000
_diffrn_orient_matrix_UB_12      0.0403814000
_diffrn_orient_matrix_UB_13      -0.0002426000
_diffrn_orient_matrix_UB_21      0.0267072000
_diffrn_orient_matrix_UB_22      0.1533127000
_diffrn_orient_matrix_UB_23      0.0392156000
_diffrn_orient_matrix_UB_31      0.0082475000
_diffrn_orient_matrix_UB_32      0.0471724000
_diffrn_orient_matrix_UB_33      -0.1271036000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4020
_diffrn_reflns_point_group_measured_fraction_full 0.704
_diffrn_reflns_point_group_measured_fraction_max 0.686
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.008
_diffrn_reflns_theta_min         5.777
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84953
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.163
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 497 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         1939
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0792P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.388
_reflns_Friedel_fraction_full    0.409
_reflns_Friedel_fraction_max     0.384
_reflns_number_gt                1856
_reflns_number_total             1939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra17209a2.cif
_cod_data_source_block           mg108_2
_cod_original_cell_volume        1451.06(10)
_cod_database_code               7226253
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         C25H30N8O10
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 O(H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C2(H2A), C13(H13), C11(H11), C10(H10), C5(H5), C4(H4), C3(H3), C12(H12)
2.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_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 1.500
_oxdiff_exptl_absorpt_empirical_full_min 0.751