#------------------------------------------------------------------------------
#$Date: 2017-09-28 04:51:33 +0300 (Thu, 28 Sep 2017) $
#$Revision: 201391 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/74/1547402.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1547402
loop_
_publ_author_name
'Cancino, Patricio'
'Paredes-Garcia, Veronica'
'Torres, Julia'
'Martínez, Sebastián'
'Kremer, Carlos'
'Spodine, Evgenia'
_publ_section_title
;
 {[Cu3Lu2(ODA)6(H2O)6]•10H2O}n . First heterometallic framework
 based on copper(II)/lutetium(III) for the catalytic oxidation of olefins
 and aromatic benzylic substrates.
;
_journal_name_full               'Catal. Sci. Technol.'
_journal_paper_doi               10.1039/C7CY01385J
_journal_year                    2017
_chemical_formula_sum            'C24 H30 Cu3 Lu2 O36'
_chemical_formula_weight         1435.05
_chemical_name_systematic        'Lutetium Copper Oxydiacetate, hydrate'
_space_group_crystal_system      hexagonal
_space_group_IT_number           192
_space_group_name_Hall           '-P 6 2c'
_space_group_name_H-M_alt        'P 6/m c c'
_symmetry_space_group_name_Hall  '-P 6 2c'
_symmetry_space_group_name_H-M   'P 6/m c c'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2017-02-09 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.021(2)
_cell_length_b                   14.021(2)
_cell_length_c                   15.713(2)
_cell_measurement_reflns_used    131
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.6144
_cell_measurement_theta_min      5.4785
_cell_volume                     2675.1(6)
_computing_cell_refinement       'APEX3 v2016.1-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v4.2.9'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER D8 venture diffractometer'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            81028
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.91
_diffrn_source                   'sealed tube'
_diffrn_source_type              'SIEMENS KFFMO2K--90C model 10190380'
_exptl_absorpt_coefficient_mu    4.920
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            'translucent pale blue'
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1382
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.765
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         1417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0224
_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/[σ²(Fo²)+(0.0119P)²+9.9425P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0590
_reflns_number_gt                989
_reflns_number_total             1417
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cy01385j2.cif
_cod_data_source_block           160416_LS_SMLuCuODAJT
_cod_original_cell_volume        2675.1(9)
_cod_database_code               1547402
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'
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
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
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'
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
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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
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_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
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)
