# Electronic Supplementary Material (ESI) for Catalysis Science & Technology.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_160416_LS_SMLuCuODAJT
_database_code_depnum_ccdc_archive 'CCDC 1532010'
_audit_update_record             
;
2017-02-09 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;
_chemical_name_systematic        'Lutetium Copper Oxydiacetate, hydrate'
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H30 Cu3 Lu2 O36'
_chemical_formula_iupac          ?
_chemical_formula_weight         1435.05

_chemical_melting_point          ?

_space_group_crystal_system      hexagonal
_space_group_name_H-M_alt        'P 6/m c c'
_space_group_name_Hall           '-P 6 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   14.021(2)
_cell_length_b                   14.021(2)
_cell_length_c                   15.713(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2675.1(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    131
_cell_measurement_theta_min      5.4785
_cell_measurement_theta_max      24.6144
_cell_measurement_temperature    293(2)

_exptl_crystal_description       hexagonal
_exptl_crystal_colour            'translucent pale blue'
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.061
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1382

_exptl_absorpt_coefficient_mu    4.920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_T_max  0.64

_exptl_special_details           
;
;

_diffrn_ambient_temperature      293(2)

_diffrn_source                   'sealed tube'
_diffrn_source_type              'SIEMENS KFFMO2K--90C model 10190380'

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'curved graphite'

_diffrn_measurement_device_type  'BRUKER D8 venture diffractometer'
_diffrn_measurement_method       ?

_diffrn_detector_area_resol_mean 10.4167

_diffrn_reflns_number            81028
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_full        30.51
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22

_refine_special_details          
;
Disordered solvent in the cavities was 
removed with solvent masking procedure in OLEX2
;

_reflns_number_total             1417
_reflns_number_gt                989
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0224
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0590
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.132
_refine_ls_number_reflns         1417
_refine_ls_number_parameters     56
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0119P)²+9.9425P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.765
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'Bruker Instrument Service v4.2.9'
_computing_cell_refinement       'APEX3 v2016.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu Lu1 0.6667 0.3333 0.75 0.02038(8) Uani d T P S 1 . .
Cu Cu1 0.5 0.5 0.5 0.02047(14) Uani d T P S 1 . .
O O1 0.76613(12) 0.5323(2) 0.75 0.0275(6) Uani d T P S 1 . .
O O1W 0.4868(4) 0.3185(3) 0.5 0.0454(10) Uani d T P S 1 . .
H H1W 0.524(8) 0.315(3) 0.461(6) 0.068 Uiso calc . . GR 0.5 . .
O O2 0.6095(2) 0.4149(2) 0.64760(14) 0.0316(5) Uani d . . . 1 . .
O O3 0.6158(2) 0.5624(2) 0.58621(17) 0.0384(6) Uani d . . . 1 . .
C C1 0.7441(4) 0.5940(3) 0.6915(3) 0.0562(13) Uani d . . . 1 . .
H H1A 0.808 0.6366 0.6557 0.067 Uiso calc . . R 1 . .
H H1B 0.7278 0.6446 0.7215 0.067 Uiso calc . . R 1 . .
C C2 0.6481(3) 0.5176(3) 0.6381(2) 0.0296(7) Uani d . . . 1 . .


_geom_special_details            
;

All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Lu1 O1 2_655 2.415(3) ?
Lu1 O1 . 2.416(3) ?
Lu1 O1 3_665 2.415(3) ?
Lu1 O2 2_655 2.336(2) ?
Lu1 O2 3_665 2.336(2) ?
Lu1 O2 11_656 2.336(2) ?
Lu1 O2 10_666 2.336(2) ?
Lu1 O2 . 2.336(2) ?
Lu1 O2 12_556 2.336(2) ?
Cu1 O1W . 2.457(4) ?
Cu1 O3 4_665 1.953(3) ?
Cu1 O3 . 1.953(3) ?
Cu1 O3 16_556 1.953(3) ?
Cu1 O3 13_666 1.953(3) ?
O1 C1 11_656 1.398(4) ?
O1 C1 . 1.398(4) ?
O1W H1W . 0.81(9) ?
O2 C2 . 1.268(4) ?
O3 C2 . 1.246(4) ?
C1 H1A . 0.97 ?
C1 H1B . 0.97 ?
C1 C2 . 1.491(5) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Lu1 O1 3_665 . 120.0000(10) ?
O1 Lu1 O1 3_665 2_655 120.0 ?
O1 Lu1 O1 2_655 . 120.0 ?
O2 Lu1 O1 10_666 2_655 64.91(6) ?
O2 Lu1 O1 3_665 . 72.71(6) ?
O2 Lu1 O1 3_665 3_665 64.91(6) ?
O2 Lu1 O1 10_666 . 72.71(6) ?
O2 Lu1 O1 11_656 3_665 72.71(6) ?
O2 Lu1 O1 12_556 3_665 64.91(6) ?
O2 Lu1 O1 10_666 3_665 136.16(6) ?
O2 Lu1 O1 . 2_655 72.71(6) ?
O2 Lu1 O1 2_655 3_665 72.71(6) ?
O2 Lu1 O1 12_556 . 136.16(6) ?
O2 Lu1 O1 12_556 2_655 72.71(6) ?
O2 Lu1 O1 2_655 . 136.16(6) ?
O2 Lu1 O1 3_665 2_655 136.16(6) ?
O2 Lu1 O1 . . 64.91(6) ?
O2 Lu1 O1 11_656 2_655 136.16(6) ?
O2 Lu1 O1 . 3_665 136.16(6) ?
O2 Lu1 O1 2_655 2_655 64.91(6) ?
O2 Lu1 O1 11_656 . 64.91(6) ?
O2 Lu1 O2 12_556 10_666 77.78(9) ?
O2 Lu1 O2 10_666 . 87.68(11) ?
O2 Lu1 O2 3_665 2_655 77.78(9) ?
O2 Lu1 O2 3_665 10_666 145.42(13) ?
O2 Lu1 O2 12_556 11_656 77.78(9) ?
O2 Lu1 O2 11_656 10_666 77.78(9) ?
O2 Lu1 O2 2_655 . 77.78(9) ?
O2 Lu1 O2 2_655 10_666 129.82(12) ?
O2 Lu1 O2 12_556 3_665 129.82(12) ?
O2 Lu1 O2 12_556 . 145.42(13) ?
O2 Lu1 O2 12_556 2_655 87.68(12) ?
O2 Lu1 O2 3_665 . 77.78(9) ?
O2 Lu1 O2 11_656 2_655 145.42(13) ?
O2 Lu1 O2 11_656 . 129.82(12) ?
O2 Lu1 O2 3_665 11_656 87.68(12) ?
O3 Cu1 O1W 16_556 . 94.56(11) ?
O3 Cu1 O1W . . 94.56(11) ?
O3 Cu1 O1W 13_666 . 85.44(11) ?
O3 Cu1 O1W 4_665 . 85.44(11) ?
O3 Cu1 O3 . 13_666 180.00(15) ?
O3 Cu1 O3 13_666 16_556 92.19(17) ?
O3 Cu1 O3 . 16_556 87.81(17) ?
O3 Cu1 O3 . 4_665 92.19(17) ?
O3 Cu1 O3 16_556 4_665 180.0 ?
O3 Cu1 O3 13_666 4_665 87.81(17) ?
C1 O1 Lu1 11_656 . 122.4(2) ?
C1 O1 Lu1 . . 122.4(2) ?
C1 O1 C1 11_656 . 115.2(4) ?
Cu1 O1W H1W . . 109.5 ?
C2 O2 Lu1 . . 125.5(2) ?
C2 O3 Cu1 . . 131.2(2) ?
O1 C1 H1A . . 109.9 ?
O1 C1 H1B . . 109.9 ?
O1 C1 C2 . . 108.9(3) ?
H1A C1 H1B . . 108.3 ?
C2 C1 H1A . . 109.9 ?
C2 C1 H1B . . 109.9 ?
O2 C2 C1 . . 118.0(3) ?
O3 C2 O2 . . 126.4(3) ?
O3 C2 C1 . . 115.6(3) ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Lu1 O1 C1 C2 . . . . 4.2(5) ?
Lu1 O2 C2 O3 . . . . -176.9(3) ?
Lu1 O2 C2 C1 . . . . 5.3(5) ?
Cu1 O3 C2 O2 . . . . -1.0(6) ?
Cu1 O3 C2 C1 . . . . 176.8(3) ?
O1 C1 C2 O2 . . . . -5.8(6) ?
O1 C1 C2 O3 . . . . 176.2(3) ?
C1 O1 C1 C2 11_656 . . . -175.8(5) ?


