#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:37:38 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180513 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/82/7218277.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_7218277
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 Gd2 N4 O12'
_chemical_formula_weight         1608.22
_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                110.75(3)
_cell_angle_beta                 96.41(3)
_cell_angle_gamma                101.87(2)
_cell_formula_units_Z            1
_cell_length_a                   10.0755(3)
_cell_length_b                   11.8866(3)
_cell_length_c                   14.3488(4)
_cell_measurement_reflns_used    23098
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.534
_cell_measurement_theta_min      4.704
_cell_volume                     1540.3(4)
_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 0.919
_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  0.0270
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23098
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         30.357
_diffrn_reflns_theta_min         1.549
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.462
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6855
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Bruker-AXS (2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_description       Plate
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         8534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0249
_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)+(0.0246P)²+0.1107P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7505
_reflns_number_total             8534
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4ce01806k2.cif
_cod_data_source_block           Compound_5
_cod_depositor_comments
'Adding full bibliography for 7218273--7218283.cif.'
_cod_database_code               7218277
#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
Gd1 Gd 0.87592(2) 0.12696(2) 0.06455(2) 0.02595(4) Uani 1 1 d . .
Cl1 Cl 0.64000(10) 0.31416(9) 0.65900(6) 0.0737(2) Uani 1 1 d . .
Cl3 Cl 1.29154(13) 0.08031(11) 0.59558(7) 0.1069(4) Uani 1 1 d . .
Cl2 Cl 1.68951(10) 0.58038(9) 0.41250(8) 0.0931(3) Uani 1 1 d . .
O1 O 0.71298(17) 0.15180(16) 0.17418(12) 0.0396(4) Uani 1 1 d . .
O2 O 0.92682(18) 0.26252(15) 0.25043(12) 0.0424(4) Uani 1 1 d . .
O6 O 0.92618(18) -0.00264(16) 0.14746(12) 0.0438(4) Uani 1 1 d . .
O4 O 1.11446(17) 0.17292(19) 0.09893(14) 0.0522(5) Uani 1 1 d . .
N2 N 0.90471(19) 0.35679(16) 0.08755(14) 0.0333(4) Uani 1 1 d . .
C25 C 1.5838(3) 0.3947(2) 0.2280(2) 0.0443(6) Uani 1 1 d . .
H25 H 1.6704 0.4160 0.2126 0.053 Uiso 1 1 calc R U
O5 O 0.92406(18) 0.11388(16) -0.09511(12) 0.0419(4) Uani 1 1 d . .
O3 O 0.73119(18) -0.07119(14) -0.04234(13) 0.0439(4) Uani 1 1 d . .
N1 N 0.67252(18) 0.17788(16) -0.03411(13) 0.0293(4) Uani 1 1 d . .
C12 C 0.6891(2) 0.2961(2) -0.03076(16) 0.0300(4) Uani 1 1 d . .
C20 C 1.2357(2) 0.1633(2) 0.10052(17) 0.0345(5) Uani 1 1 d . .
C27 C 1.0261(2) -0.0461(2) 0.16317(17) 0.0324(5) Uani 1 1 d . .
C14 C 0.7617(3) 0.2484(2) 0.35555(17) 0.0387(5) Uani 1 1 d . .
C13 C 0.8030(3) 0.2204(2) 0.25448(17) 0.0341(5) Uani 1 1 d . .
C11 C 0.8104(2) 0.3909(2) 0.03520(16) 0.0320(5) Uani 1 1 d . .
C26 C 1.4787(2) 0.2969(2) 0.15689(18) 0.0356(5) Uani 1 1 d . .
H26 H 1.4958 0.2505 0.0942 0.043 Uiso 1 1 calc R U
C21 C 1.3491(2) 0.2679(2) 0.17842(16) 0.0313(5) Uani 1 1 d . .
C7 C 0.8253(3) 0.5156(2) 0.04504(19) 0.0412(6) Uani 1 1 d . .
C28 C 1.0906(2) -0.0152(2) 0.27192(17) 0.0352(5) Uani 1 1 d . .
C4 C 0.5910(3) 0.3298(2) -0.08636(18) 0.0379(5) Uani 1 1 d . .
C3 C 0.4715(3) 0.2363(3) -0.14587(19) 0.0476(6) Uani 1 1 d . .
H3 H 0.4045 0.2546 -0.1841 0.057 Uiso 1 1 calc R U
C5 C 0.6147(3) 0.4560(3) -0.0781(2) 0.0506(7) Uani 1 1 d . .
H5 H 0.5521 0.4768 -0.1177 0.061 Uiso 1 1 calc R U
C17 C 0.6879(3) 0.2918(3) 0.5419(2) 0.0529(7) Uani 1 1 d . .
C10 C 1.0127(3) 0.4460(2) 0.15166(19) 0.0429(6) Uani 1 1 d . .
H10 H 1.0775 0.4238 0.1882 0.052 Uiso 1 1 calc R U
C22 C 1.3247(3) 0.3352(2) 0.27301(19) 0.0450(6) Uani 1 1 d . .
H22 H 1.2372 0.3169 0.2878 0.054 Uiso 1 1 calc R U
C1 C 0.5572(2) 0.0932(2) -0.09118(17) 0.0357(5) Uani 1 1 d . .
H1 H 0.5446 0.0123 -0.0938 0.043 Uiso 1 1 calc R U
C33 C 1.2023(3) -0.0595(3) 0.2937(2) 0.0495(6) Uani 1 1 d . .
H33 H 1.2357 -0.1102 0.2410 0.059 Uiso 1 1 calc R U
C16 C 0.5875(3) 0.2270(3) 0.4545(2) 0.0531(7) Uani 1 1 d . .
H16 H 0.4958 0.1981 0.4580 0.064 Uiso 1 1 calc R U
C19 C 0.8599(3) 0.3149(3) 0.4449(2) 0.0537(7) Uani 1 1 d . .
H19 H 0.9514 0.3451 0.4418 0.064 Uiso 1 1 calc R U
C24 C 1.5582(3) 0.4592(2) 0.3210(2) 0.0508(7) Uani 1 1 d . .
C8 C 0.9412(3) 0.6055(2) 0.1135(2) 0.0539(7) Uani 1 1 d . .
H8 H 0.9547 0.6887 0.1223 0.065 Uiso 1 1 calc R U
C18 C 0.8232(3) 0.3367(3) 0.5387(2) 0.0647(9) Uani 1 1 d . .
H18 H 0.8893 0.3811 0.5985 0.078 Uiso 1 1 calc R U
C29 C 1.0422(3) 0.0593(3) 0.3507(2) 0.0534(7) Uani 1 1 d . .
H29 H 0.9672 0.0892 0.3367 0.064 Uiso 1 1 calc R U
C15 C 0.6260(3) 0.2059(2) 0.36150(19) 0.0457(6) Uani 1 1 d . .
H15 H 0.5593 0.1622 0.3019 0.055 Uiso 1 1 calc R U
C9 C 1.0337(3) 0.5716(2) 0.1669(2) 0.0538(7) Uani 1 1 d . .
H9 H 1.1102 0.6312 0.2132 0.065 Uiso 1 1 calc R U
C32 C 1.2643(3) -0.0282(3) 0.3940(2) 0.0652(9) Uani 1 1 d . .
H32 H 1.3399 -0.0569 0.4088 0.078 Uiso 1 1 calc R U
C23 C 1.4312(3) 0.4297(3) 0.3453(2) 0.0578(8) Uani 1 1 d . .
H23 H 1.4167 0.4729 0.4097 0.069 Uiso 1 1 calc R U
C2 C 0.4532(3) 0.1187(3) -0.14780(19) 0.0459(6) Uani 1 1 d . .
H2 H 0.3733 0.0564 -0.1860 0.055 Uiso 1 1 calc R U
C6 C 0.7247(3) 0.5448(2) -0.0149(2) 0.0522(7) Uani 1 1 d . .
H6 H 0.7362 0.6266 -0.0098 0.063 Uiso 1 1 calc R U
C31 C 1.2136(3) 0.0451(3) 0.4706(2) 0.0606(8) Uani 1 1 d . .
C30 C 1.1043(4) 0.0903(3) 0.4510(2) 0.0662(9) Uani 1 1 d . .
H30 H 1.0718 0.1411 0.5041 0.079 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'
Gd Gd -0.1653 3.9035 '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 Gd1 O6 75.49(6) . .
O4 Gd1 O5 79.04(6) . .
O6 Gd1 O5 125.22(6) . .
O4 Gd1 O3 123.73(6) . .
O6 Gd1 O3 76.59(6) . .
O5 Gd1 O3 78.82(6) . .
O4 Gd1 O1 131.60(6) . .
O6 Gd1 O1 80.81(6) . .
O5 Gd1 O1 146.90(6) . .
O3 Gd1 O1 89.72(6) . .
O4 Gd1 O2 79.72(6) . .
O6 Gd1 O2 75.23(6) . .
O5 Gd1 O2 144.74(6) . .
O3 Gd1 O2 136.41(6) . .
O1 Gd1 O2 53.46(6) . .
O4 Gd1 N2 86.89(6) . .
O6 Gd1 N2 143.63(6) . .
O5 Gd1 N2 80.64(6) . .
O3 Gd1 N2 138.24(6) . .
O1 Gd1 N2 88.07(6) . .
O2 Gd1 N2 70.40(6) . .
O4 Gd1 N1 140.18(6) . .
O6 Gd1 N1 143.92(6) . .
O5 Gd1 N1 71.36(5) . .
O3 Gd1 N1 76.23(5) . .
O1 Gd1 N1 75.78(5) . .
O2 Gd1 N1 110.31(5) . .
N2 Gd1 N1 62.83(6) . .
O4 Gd1 C13 105.20(7) . .
O6 Gd1 C13 74.38(6) . .
O5 Gd1 C13 160.03(6) . .
O3 Gd1 C13 112.76(7) . .
O1 Gd1 C13 26.86(6) . .
O2 Gd1 C13 26.76(6) . .
N2 Gd1 C13 80.13(6) . .
N1 Gd1 C13 94.94(6) . .
C13 O1 Gd1 94.93(14) . .
C13 O2 Gd1 89.70(13) . .
C27 O6 Gd1 136.47(15) . .
C20 O4 Gd1 162.42(18) . .
C10 N2 C11 117.7(2) . .
C10 N2 Gd1 120.83(15) . .
C11 N2 Gd1 121.51(14) . .
C24 C25 C26 119.0(2) . .
C24 C25 H25 120.5 . .
C26 C25 H25 120.5 . .
C27 O5 Gd1 137.53(14) 2_755 .
C20 O3 Gd1 128.42(15) 2_755 .
C1 N1 C12 117.41(18) . .
C1 N1 Gd1 123.70(14) . .
C12 N1 Gd1 118.81(14) . .
N1 C12 C4 122.8(2) . .
N1 C12 C11 118.17(19) . .
C4 C12 C11 119.0(2) . .
O4 C20 O3 124.4(2) . 2_755
O4 C20 C21 117.8(2) . .
O3 C20 C21 117.8(2) 2_755 .
O5 C27 O6 125.0(2) 2_755 .
O5 C27 C28 117.4(2) 2_755 .
O6 C27 C28 117.6(2) . .
C15 C14 C19 118.9(2) . .
C15 C14 C13 120.6(2) . .
C19 C14 C13 120.5(2) . .
O2 C13 O1 121.2(2) . .
O2 C13 C14 119.7(2) . .
O1 C13 C14 119.1(2) . .
O2 C13 Gd1 63.54(12) . .
O1 C13 Gd1 58.20(11) . .
C14 C13 Gd1 170.20(15) . .
N2 C11 C7 122.5(2) . .
N2 C11 C12 118.29(19) . .
C7 C11 C12 119.2(2) . .
C21 C26 C25 120.5(2) . .
C21 C26 H26 119.7 . .
C25 C26 H26 119.7 . .
C26 C21 C22 119.7(2) . .
C26 C21 C20 120.1(2) . .
C22 C21 C20 120.3(2) . .
C8 C7 C11 117.3(2) . .
C8 C7 C6 123.0(2) . .
C11 C7 C6 119.8(2) . .
C29 C28 C33 119.3(2) . .
C29 C28 C27 120.7(2) . .
C33 C28 C27 120.0(2) . .
C3 C4 C12 117.3(2) . .
C3 C4 C5 123.0(2) . .
C12 C4 C5 119.7(2) . .
C2 C3 C4 120.0(2) . .
C2 C3 H3 120.0 . .
C4 C3 H3 120.0 . .
C6 C5 C4 121.5(2) . .
C6 C5 H5 119.3 . .
C4 C5 H5 119.3 . .
C18 C17 C16 121.8(2) . .
C18 C17 Cl1 119.7(2) . .
C16 C17 Cl1 118.4(2) . .
N2 C10 C9 123.3(2) . .
N2 C10 H10 118.4 . .
C9 C10 H10 118.4 . .
C23 C22 C21 119.7(2) . .
C23 C22 H22 120.1 . .
C21 C22 H22 120.1 . .
N1 C1 C2 123.7(2) . .
N1 C1 H1 118.2 . .
C2 C1 H1 118.2 . .
C28 C33 C32 120.0(3) . .
C28 C33 H33 120.0 . .
C32 C33 H33 120.0 . .
C17 C16 C15 118.5(3) . .
C17 C16 H16 120.7 . .
C15 C16 H16 120.7 . .
C18 C19 C14 120.7(3) . .
C18 C19 H19 119.6 . .
C14 C19 H19 119.6 . .
C25 C24 C23 121.5(2) . .
C25 C24 Cl2 119.9(2) . .
C23 C24 Cl2 118.6(2) . .
C9 C8 C7 120.1(2) . .
C9 C8 H8 119.9 . .
C7 C8 H8 119.9 . .
C17 C18 C19 118.9(3) . .
C17 C18 H18 120.6 . .
C19 C18 H18 120.6 . .
C28 C29 C30 120.6(3) . .
C28 C29 H29 119.7 . .
C30 C29 H29 119.7 . .
C14 C15 C16 121.1(3) . .
C14 C15 H15 119.4 . .
C16 C15 H15 119.4 . .
C8 C9 C10 119.1(2) . .
C8 C9 H9 120.4 . .
C10 C9 H9 120.4 . .
C31 C32 C33 119.5(3) . .
C31 C32 H32 120.2 . .
C33 C32 H32 120.2 . .
C24 C23 C22 119.5(3) . .
C24 C23 H23 120.2 . .
C22 C23 H23 120.2 . .
C3 C2 C1 118.7(2) . .
C3 C2 H2 120.6 . .
C1 C2 H2 120.6 . .
C5 C6 C7 120.8(2) . .
C5 C6 H6 119.6 . .
C7 C6 H6 119.6 . .
C32 C31 C30 121.5(3) . .
C32 C31 Cl3 118.4(2) . .
C30 C31 Cl3 120.1(3) . .
C31 C30 C29 119.1(3) . .
C31 C30 H30 120.4 . .
C29 C30 H30 120.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Gd1 O4 2.3069(16) .
Gd1 O6 2.3516(16) .
Gd1 O5 2.3526(15) .
Gd1 O3 2.3567(16) .
Gd1 O1 2.3883(15) .
Gd1 O2 2.5063(16) .
Gd1 N2 2.5826(18) .
Gd1 N1 2.6534(17) .
Gd1 C13 2.800(2) .
Cl1 C17 1.745(3) .
Cl3 C31 1.739(3) .
Cl2 C24 1.743(3) .
O1 C13 1.270(3) .
O2 C13 1.261(3) .
O6 C27 1.256(3) .
O4 C20 1.249(3) .
N2 C10 1.329(3) .
N2 C11 1.359(3) .
C25 C24 1.367(4) .
C25 C26 1.388(3) .
C25 H25 0.9300 .
O5 C27 1.254(3) 2_755
O3 C20 1.253(3) 2_755
N1 C1 1.325(3) .
N1 C12 1.363(3) .
C12 C4 1.410(3) .
C12 C11 1.442(3) .
C20 O3 1.253(3) 2_755
C20 C21 1.499(3) .
C27 O5 1.254(3) 2_755
C27 C28 1.504(3) .
C14 C15 1.380(4) .
C14 C19 1.388(4) .
C14 C13 1.496(3) .
C11 C7 1.412(3) .
C26 C21 1.378(3) .
C26 H26 0.9300 .
C21 C22 1.389(3) .
C7 C8 1.398(4) .
C7 C6 1.431(4) .
C28 C29 1.376(3) .
C28 C33 1.387(3) .
C4 C3 1.400(4) .
C4 C5 1.429(3) .
C3 C2 1.363(4) .
C3 H3 0.9300 .
C5 C6 1.334(4) .
C5 H5 0.9300 .
C17 C18 1.370(4) .
C17 C16 1.379(4) .
C10 C9 1.396(3) .
C10 H10 0.9300 .
C22 C23 1.385(4) .
C22 H22 0.9300 .
C1 C2 1.401(3) .
C1 H1 0.9300 .
C33 C32 1.387(4) .
C33 H33 0.9300 .
C16 C15 1.383(4) .
C16 H16 0.9300 .
C19 C18 1.385(4) .
C19 H19 0.9300 .
C24 C23 1.372(4) .
C8 C9 1.354(4) .
C8 H8 0.9300 .
C18 H18 0.9300 .
C29 C30 1.387(4) .
C29 H29 0.9300 .
C15 H15 0.9300 .
C9 H9 0.9300 .
C32 C31 1.364(4) .
C32 H32 0.9300 .
C23 H23 0.9300 .
C2 H2 0.9300 .
C6 H6 0.9300 .
C31 C30 1.365(4) .
C30 H30 0.9300 .
