#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:37:38 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180513 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/82/7218282.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_7218282
loop_
_publ_author_name
'Carter, Korey P.'
'Zulato, Cecília H. F.'
'Cahill, Christopher L.'
_publ_section_title
;
 Exploring supramolecular assembly and luminescent behavior in a series of
 RE-p-chlorobenzoic acid-1,10-phenanthroline complexes
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              10189
_journal_paper_doi               10.1039/C4CE01806K
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C66 H40 Cl6 Lu2 N4 O12'
_chemical_formula_weight         1643.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                111.419(3)
_cell_angle_beta                 96.559(3)
_cell_angle_gamma                101.088(2)
_cell_formula_units_Z            1
_cell_length_a                   10.1082(5)
_cell_length_b                   11.7926(5)
_cell_length_c                   14.2440(7)
_cell_measurement_reflns_used    21080
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      40.334
_cell_measurement_theta_min      4.702
_cell_volume                     1519.19(13)
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_collection       'APEX, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_molecular_graphics    'Crystal Maker (Palmer, 2009)'
_computing_publication_material  'WINGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21078
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.052
_diffrn_reflns_theta_min         1.568
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.562
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6741
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Bruker-AXS (2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_description       Plate
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.956
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0407
_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/[σ²(Fo²)+(0.0174P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0661
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5578
_reflns_number_total             7367
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4ce01806k2.cif
_cod_data_source_block           Compound_10
_cod_depositor_comments
'Adding full bibliography for 7218273--7218283.cif.'
_cod_database_code               7218282
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Lu1 Lu 0.37838(2) 0.12888(2) 0.56466(2) 0.02654(6) Uani 1 1 d . .
Cl1 Cl 0.13514(17) 0.31175(16) 1.15729(11) 0.0728(5) Uani 1 1 d . .
Cl2 Cl 1.18809(17) 0.57646(15) 0.90857(13) 0.0872(6) Uani 1 1 d . .
Cl3 Cl 0.7867(2) 0.08203(19) 1.09797(13) 0.1077(7) Uani 1 1 d . .
O2 O 0.4286(4) 0.2630(3) 0.7488(2) 0.0429(9) Uani 1 1 d . .
O5 O 0.4301(3) 0.0036(3) 0.6448(2) 0.0425(8) Uani 1 1 d . .
O1 O 0.2184(3) 0.1497(3) 0.6693(2) 0.0381(8) Uani 1 1 d . .
O4 O 0.6078(3) 0.1781(3) 0.5991(2) 0.0461(9) Uani 1 1 d . .
C25 C 1.0741(5) 0.3896(5) 0.7234(4) 0.0458(13) Uani 1 1 d . .
H25 H 1.1588 0.4099 0.7060 0.055 Uiso 1 1 calc R U
N2 N 0.4095(4) 0.3532(3) 0.5879(3) 0.0318(9) Uani 1 1 d . .
O6 O 0.4225(3) 0.1126(3) 0.4087(2) 0.0414(8) Uani 1 1 d . .
O3 O 0.2445(3) -0.0651(3) 0.4604(2) 0.0399(8) Uani 1 1 d . .
C14 C 0.2617(5) 0.2478(4) 0.8524(4) 0.0361(11) Uani 1 1 d . .
C20 C 0.7265(5) 0.1616(4) 0.5988(4) 0.0319(11) Uani 1 1 d . .
N1 N 0.1779(4) 0.1750(3) 0.4678(3) 0.0295(9) Uani 1 1 d . .
C12 C 0.1927(5) 0.2936(4) 0.4721(3) 0.0280(10) Uani 1 1 d . .
C28 C 0.5893(5) -0.0149(4) 0.7705(4) 0.0337(11) Uani 1 1 d . .
C11 C 0.3138(5) 0.3884(4) 0.5366(3) 0.0289(10) Uani 1 1 d . .
C13 C 0.3067(5) 0.2205(4) 0.7514(4) 0.0343(12) Uani 1 1 d . .
C27 C 0.5265(5) -0.0434(4) 0.6608(4) 0.0318(11) Uani 1 1 d . .
C1 C 0.0621(5) 0.0906(4) 0.4118(3) 0.0362(12) Uani 1 1 d . .
H1 H 0.0496 0.0096 0.4101 0.043 Uiso 1 1 calc R U
C21 C 0.8417(4) 0.2649(4) 0.6764(3) 0.0284(10) Uani 1 1 d . .
C5 C 0.1160(6) 0.4548(5) 0.4251(4) 0.0506(15) Uani 1 1 d . .
H5 H 0.0520 0.4763 0.3867 0.061 Uiso 1 1 calc R U
C3 C -0.0256(5) 0.2338(5) 0.3568(4) 0.0464(14) Uani 1 1 d . .
H3 H -0.0930 0.2526 0.3191 0.056 Uiso 1 1 calc R U
C15 C 0.1273(5) 0.2046(5) 0.8569(4) 0.0453(13) Uani 1 1 d . .
H15 H 0.0620 0.1603 0.7961 0.054 Uiso 1 1 calc R U
C17 C 0.1839(6) 0.2896(5) 1.0386(4) 0.0526(15) Uani 1 1 d . .
C16 C 0.0875(6) 0.2257(5) 0.9502(4) 0.0483(14) Uani 1 1 d . .
H16 H -0.0039 0.1967 0.9524 0.058 Uiso 1 1 calc R U
C4 C 0.0945(5) 0.3269(4) 0.4159(3) 0.0344(11) Uani 1 1 d . .
C7 C 0.3292(5) 0.5148(4) 0.5468(4) 0.0379(12) Uani 1 1 d . .
C18 C 0.3189(6) 0.3373(6) 1.0378(4) 0.0607(17) Uani 1 1 d . .
H18 H 0.3829 0.3830 1.0992 0.073 Uiso 1 1 calc R U
C29 C 0.5408(6) 0.0611(5) 0.8507(4) 0.0529(15) Uani 1 1 d . .
H29 H 0.4667 0.0927 0.8370 0.064 Uiso 1 1 calc R U
C26 C 0.9696(5) 0.2925(4) 0.6522(4) 0.0374(12) Uani 1 1 d . .
H26 H 0.9851 0.2454 0.5880 0.045 Uiso 1 1 calc R U
C22 C 0.8219(5) 0.3337(5) 0.7732(4) 0.0456(13) Uani 1 1 d . .
H22 H 0.7363 0.3166 0.7903 0.055 Uiso 1 1 calc R U
C10 C 0.5172(5) 0.4424(4) 0.6518(4) 0.0408(12) Uani 1 1 d . .
H10 H 0.5822 0.4194 0.6880 0.049 Uiso 1 1 calc R U
C8 C 0.4448(6) 0.6043(5) 0.6150(4) 0.0487(14) Uani 1 1 d . .
H8 H 0.4581 0.6884 0.6247 0.058 Uiso 1 1 calc R U
C6 C 0.2272(6) 0.5439(5) 0.4884(4) 0.0512(15) Uani 1 1 d . .
H6 H 0.2377 0.6264 0.4941 0.061 Uiso 1 1 calc R U
C33 C 0.7020(5) -0.0572(5) 0.7930(4) 0.0506(14) Uani 1 1 d . .
H33 H 0.7377 -0.1062 0.7395 0.061 Uiso 1 1 calc R U
C31 C 0.7104(7) 0.0460(6) 0.9723(4) 0.0627(17) Uani 1 1 d . .
C30 C 0.6021(7) 0.0905(5) 0.9516(4) 0.0653(18) Uani 1 1 d . .
H30 H 0.5684 0.1412 1.0054 0.078 Uiso 1 1 calc R U
C19 C 0.3582(6) 0.3159(5) 0.9435(4) 0.0537(15) Uani 1 1 d . .
H19 H 0.4491 0.3473 0.9415 0.064 Uiso 1 1 calc R U
C2 C -0.0427(5) 0.1155(5) 0.3551(4) 0.0450(13) Uani 1 1 d . .
H2 H -0.1221 0.0528 0.3171 0.054 Uiso 1 1 calc R U
C24 C 1.0546(5) 0.4558(5) 0.8184(4) 0.0497(15) Uani 1 1 d . .
C9 C 0.5382(6) 0.5685(5) 0.6676(4) 0.0523(15) Uani 1 1 d . .
H9 H 0.6153 0.6278 0.7136 0.063 Uiso 1 1 calc R U
C23 C 0.9297(6) 0.4284(5) 0.8450(4) 0.0553(15) Uani 1 1 d . .
H23 H 0.9174 0.4731 0.9109 0.066 Uiso 1 1 calc R U
C32 C 0.7630(6) -0.0277(6) 0.8940(5) 0.0679(18) Uani 1 1 d . .
H32 H 0.8383 -0.0574 0.9086 0.081 Uiso 1 1 calc R U
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'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O4 Lu1 O6 79.29(11) . .
O4 Lu1 O3 124.05(11) . .
O6 Lu1 O3 78.14(11) . .
O4 Lu1 O5 76.19(12) . .
O6 Lu1 O5 124.62(11) . .
O3 Lu1 O5 76.07(11) . .
O4 Lu1 O1 132.35(11) . .
O6 Lu1 O1 146.23(11) . .
O3 Lu1 O1 88.92(12) . .
O5 Lu1 O1 80.86(11) . .
O4 Lu1 O2 78.84(11) . .
O6 Lu1 O2 145.37(11) . .
O3 Lu1 O2 136.49(11) . .
O5 Lu1 O2 74.98(11) . .
O1 Lu1 O2 54.94(11) . .
O4 Lu1 N2 84.21(12) . .
O6 Lu1 N2 80.70(11) . .
O3 Lu1 N2 139.90(12) . .
O5 Lu1 N2 143.08(12) . .
O1 Lu1 N2 90.17(11) . .
O2 Lu1 N2 70.67(11) . .
O4 Lu1 N1 140.05(12) . .
O6 Lu1 N1 71.64(11) . .
O3 Lu1 N1 76.30(11) . .
O5 Lu1 N1 143.37(12) . .
O1 Lu1 N1 75.04(11) . .
O2 Lu1 N1 110.99(11) . .
N2 Lu1 N1 64.81(12) . .
O4 Lu1 C13 104.98(14) . .
O6 Lu1 C13 160.80(12) . .
O3 Lu1 C13 112.71(14) . .
O5 Lu1 C13 74.32(12) . .
O1 Lu1 C13 27.81(12) . .
O2 Lu1 C13 27.27(12) . .
N2 Lu1 C13 81.14(12) . .
N1 Lu1 C13 94.92(12) . .
C13 O2 Lu1 88.7(3) . .
C27 O5 Lu1 138.9(3) . .
C13 O1 Lu1 94.4(3) . .
C20 O4 Lu1 158.1(3) . .
C24 C25 C26 120.6(5) . .
C24 C25 H25 119.7 . .
C26 C25 H25 119.7 . .
C10 N2 C11 117.7(4) . .
C10 N2 Lu1 121.5(3) . .
C11 N2 Lu1 120.7(3) . .
C27 O6 Lu1 137.9(3) 2_656 .
C20 O3 Lu1 131.6(3) 2_656 .
C15 C14 C19 119.1(5) . .
C15 C14 C13 121.4(4) . .
C19 C14 C13 119.5(5) . .
O4 C20 O3 125.2(4) . 2_656
O4 C20 C21 116.8(4) . .
O3 C20 C21 118.0(4) 2_656 .
C1 N1 C12 117.2(4) . .
C1 N1 Lu1 124.9(3) . .
C12 N1 Lu1 117.9(3) . .
N1 C12 C4 122.6(4) . .
N1 C12 C11 118.4(4) . .
C4 C12 C11 119.0(4) . .
C29 C28 C33 118.7(5) . .
C29 C28 C27 120.4(4) . .
C33 C28 C27 120.8(4) . .
N2 C11 C7 122.2(4) . .
N2 C11 C12 118.0(4) . .
C7 C11 C12 119.8(4) . .
O2 C13 O1 121.3(4) . .
O2 C13 C14 120.5(4) . .
O1 C13 C14 118.1(5) . .
O2 C13 Lu1 64.1(3) . .
O1 C13 Lu1 57.7(2) . .
C14 C13 Lu1 170.1(3) . .
O5 C27 O6 124.8(4) . 2_656
O5 C27 C28 118.4(4) . .
O6 C27 C28 116.8(4) 2_656 .
N1 C1 C2 124.2(4) . .
N1 C1 H1 117.9 . .
C2 C1 H1 117.9 . .
C22 C21 C26 119.1(4) . .
C22 C21 C20 120.4(4) . .
C26 C21 C20 120.5(4) . .
C6 C5 C4 121.0(5) . .
C6 C5 H5 119.5 . .
C4 C5 H5 119.5 . .
C2 C3 C4 119.5(5) . .
C2 C3 H3 120.2 . .
C4 C3 H3 120.2 . .
C14 C15 C16 121.1(5) . .
C14 C15 H15 119.4 . .
C16 C15 H15 119.4 . .
C16 C17 C18 121.8(5) . .
C16 C17 Cl1 119.2(5) . .
C18 C17 Cl1 119.0(4) . .
C17 C16 C15 119.0(5) . .
C17 C16 H16 120.5 . .
C15 C16 H16 120.5 . .
C3 C4 C12 117.9(4) . .
C3 C4 C5 122.4(5) . .
C12 C4 C5 119.7(5) . .
C8 C7 C11 117.4(4) . .
C8 C7 C6 123.5(5) . .
C11 C7 C6 119.1(5) . .
C17 C18 C19 118.8(5) . .
C17 C18 H18 120.6 . .
C19 C18 H18 120.6 . .
C28 C29 C30 120.1(5) . .
C28 C29 H29 119.9 . .
C30 C29 H29 119.9 . .
C25 C26 C21 120.0(5) . .
C25 C26 H26 120.0 . .
C21 C26 H26 120.0 . .
C21 C22 C23 120.0(5) . .
C21 C22 H22 120.0 . .
C23 C22 H22 120.0 . .
N2 C10 C9 123.5(5) . .
N2 C10 H10 118.3 . .
C9 C10 H10 118.3 . .
C9 C8 C7 119.8(5) . .
C9 C8 H8 120.1 . .
C7 C8 H8 120.1 . .
C5 C6 C7 121.4(5) . .
C5 C6 H6 119.3 . .
C7 C6 H6 119.3 . .
C28 C33 C32 121.0(5) . .
C28 C33 H33 119.5 . .
C32 C33 H33 119.5 . .
C30 C31 C32 120.8(5) . .
C30 C31 Cl3 120.5(5) . .
C32 C31 Cl3 118.7(5) . .
C31 C30 C29 120.4(6) . .
C31 C30 H30 119.8 . .
C29 C30 H30 119.8 . .
C14 C19 C18 120.0(5) . .
C14 C19 H19 120.0 . .
C18 C19 H19 120.0 . .
C3 C2 C1 118.5(5) . .
C3 C2 H2 120.8 . .
C1 C2 H2 120.8 . .
C25 C24 C23 120.5(5) . .
C25 C24 Cl2 120.3(4) . .
C23 C24 Cl2 119.2(5) . .
C8 C9 C10 119.3(5) . .
C8 C9 H9 120.3 . .
C10 C9 H9 120.3 . .
C24 C23 C22 119.7(5) . .
C24 C23 H23 120.1 . .
C22 C23 H23 120.1 . .
C31 C32 C33 119.0(6) . .
C31 C32 H32 120.5 . .
C33 C32 H32 120.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Lu1 O4 2.230(3) .
Lu1 O6 2.263(3) .
Lu1 O3 2.267(3) .
Lu1 O5 2.269(3) .
Lu1 O1 2.309(3) .
Lu1 O2 2.449(3) .
Lu1 N2 2.495(3) .
Lu1 N1 2.577(3) .
Lu1 C13 2.722(5) .
Cl1 C17 1.757(5) .
Cl2 C24 1.739(5) .
Cl3 C31 1.727(6) .
O2 C13 1.248(5) .
O5 C27 1.248(5) .
O1 C13 1.274(5) .
O4 C20 1.252(5) .
C25 C24 1.351(7) .
C25 C26 1.378(6) .
C25 H25 0.9300 .
N2 C10 1.324(5) .
N2 C11 1.363(5) .
O6 C27 1.265(5) 2_656
O3 C20 1.255(5) 2_656
C14 C15 1.373(6) .
C14 C19 1.389(6) .
C14 C13 1.499(6) .
C20 O3 1.255(5) 2_656
C20 C21 1.496(6) .
N1 C1 1.325(5) .
N1 C12 1.354(5) .
C12 C4 1.407(6) .
C12 C11 1.435(6) .
C28 C29 1.377(6) .
C28 C33 1.378(6) .
C28 C27 1.505(6) .
C11 C7 1.419(6) .
C27 O6 1.265(5) 2_656
C1 C2 1.399(6) .
C1 H1 0.9300 .
C21 C22 1.382(6) .
C21 C26 1.385(6) .
C5 C6 1.342(7) .
C5 C4 1.437(6) .
C5 H5 0.9300 .
C3 C2 1.363(6) .
C3 C4 1.402(6) .
C3 H3 0.9300 .
C15 C16 1.381(6) .
C15 H15 0.9300 .
C17 C16 1.360(7) .
C17 C18 1.376(7) .
C16 H16 0.9300 .
C7 C8 1.393(7) .
C7 C6 1.423(6) .
C18 C19 1.392(7) .
C18 H18 0.9300 .
C29 C30 1.386(7) .
C29 H29 0.9300 .
C26 H26 0.9300 .
C22 C23 1.386(6) .
C22 H22 0.9300 .
C10 C9 1.390(6) .
C10 H10 0.9300 .
C8 C9 1.361(7) .
C8 H8 0.9300 .
C6 H6 0.9300 .
C33 C32 1.387(7) .
C33 H33 0.9300 .
C31 C30 1.350(8) .
C31 C32 1.373(8) .
C30 H30 0.9300 .
C19 H19 0.9300 .
C2 H2 0.9300 .
C24 C23 1.373(7) .
C9 H9 0.9300 .
C23 H23 0.9300 .
C32 H32 0.9300 .
