#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/78/2217879.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2217879
loop_
_publ_author_name
'Wang, Shou-Bin'
'He, Hong-Mei'
'Li, Sheng'
'Tang, Kun'
_publ_section_title
Tetrakis(μ-2,4-difluorobenzoato)bis[(2,4-difluorobenzoato)(1,10-phenanthroline)gadolinium(III)]
_journal_coeditor_code           CF2184
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m516
_journal_paper_doi               10.1107/S1600536808004431
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Gd2 (C7 H3 F2 O2)6 (C12 H8 N2)2]'
_chemical_formula_moiety         'C66 H34 F12 Gd2 N4 O12'
_chemical_formula_sum            'C66 H34 F12 Gd2 N4 O12'
_chemical_formula_weight         1617.47
_chemical_name_systematic
;
Tetrakis(μ-2,4-difluorobenzoato)bis[(2,4-difluorobenzoato)(1,10-
phenanthroline)gadolinium(III)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.364(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.132(3)
_cell_length_b                   13.663(3)
_cell_length_c                   15.286(3)
_cell_measurement_reflns_used    5535
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      2.05
_cell_volume                     2981.6(11)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15634
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.312
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.692
_refine_diff_density_min         -0.639
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0528P)²+4.39P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0946
_reflns_number_gt                4598
_reflns_number_total             5535
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cf2184.cif
_cod_data_source_block           I
_cod_original_cell_volume        2981.6(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2217879
_cod_database_fobs_code          2217879
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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
_atom_site_occupancy
Gd Gd1 0.997885(14) 0.144628(14) 0.957975(13) 0.02862(9) Uani d . 1
C C1 1.1346(3) 0.2166(3) 0.8849(3) 0.0373(10) Uani d . 1
C C2 1.2110(3) 0.2446(3) 0.8476(3) 0.0428(11) Uani d . 1
C C3 1.1982(4) 0.2280(4) 0.7539(4) 0.0530(13) Uani d . 1
H H3 1.1411 0.2041 0.7152 0.064 Uiso calc R 1
C C4 1.2694(5) 0.2467(5) 0.7181(4) 0.0725(19) Uani d . 1
H H4 1.2606 0.2353 0.6558 0.087 Uiso calc R 1
C C5 1.3513(5) 0.2816(5) 0.7747(5) 0.076(2) Uani d . 1
C C6 1.3667(5) 0.2995(6) 0.8637(6) 0.095(3) Uani d . 1
H H6 1.4243 0.3240 0.9009 0.113 Uiso calc R 1
C C7 1.2965(4) 0.2815(5) 0.9009(4) 0.0667(17) Uani d . 1
C C8 0.9247(3) -0.0549(3) 0.8221(3) 0.0316(9) Uani d . 1
C C9 0.9086(3) -0.0732(3) 0.7207(3) 0.0328(9) Uani d . 1
C C10 0.9380(3) -0.0029(3) 0.6705(3) 0.0413(11) Uani d . 1
H H10 0.9713 0.0512 0.7013 0.050 Uiso calc R 1
C C11 0.9189(4) -0.0117(4) 0.5764(3) 0.0573(14) Uani d . 1
H H11 0.9399 0.0351 0.5437 0.069 Uiso calc R 1
C C12 0.8686(5) -0.0904(5) 0.5324(3) 0.0656(17) Uani d . 1
C C13 0.8377(4) -0.1626(4) 0.5768(3) 0.0541(14) Uani d . 1
H H13 0.8030 -0.2153 0.5446 0.065 Uiso calc R 1
C C14 0.8605(3) -0.1536(3) 0.6721(3) 0.0407(11) Uani d . 1
C C15 0.8390(3) 0.0592(3) 1.0120(3) 0.0344(9) Uani d . 1
C C16 0.7585(3) 0.0448(3) 1.0482(3) 0.0422(11) Uani d . 1
C C17 0.7753(5) 0.0095(4) 1.1374(4) 0.0631(16) Uani d . 1
H H17 0.8347 -0.0130 1.1717 0.076 Uiso calc R 1
C C18 0.7040(6) 0.0075(5) 1.1760(5) 0.085(2) Uani d . 1
H H18 0.7150 -0.0182 1.2350 0.102 Uiso calc R 1
C C19 0.6197(6) 0.0427(6) 1.1277(6) 0.092(3) Uani d . 1
C C20 0.5978(4) 0.0755(5) 1.0382(5) 0.0761(19) Uani d . 1
H H20 0.5378 0.0968 1.0048 0.091 Uiso calc R 1
C C21 0.6685(4) 0.0755(4) 0.9998(4) 0.0532(13) Uani d . 1
C C22 0.9877(4) 0.3346(4) 1.1111(3) 0.0454(12) Uani d . 1
H H22 1.0244 0.2895 1.1532 0.054 Uiso calc R 1
C C23 0.9628(4) 0.4212(4) 1.1453(4) 0.0553(14) Uani d . 1
H H23 0.9809 0.4318 1.2089 0.066 Uiso calc R 1
C C24 0.9121(4) 0.4896(4) 1.0857(4) 0.0548(14) Uani d . 1
H H24 0.8961 0.5479 1.1082 0.066 Uiso calc R 1
C C25 0.8838(3) 0.4726(3) 0.9899(4) 0.0440(11) Uani d . 1
C C26 0.9099(3) 0.3819(3) 0.9608(3) 0.0371(10) Uani d . 1
C C27 0.8324(4) 0.5425(4) 0.9223(4) 0.0569(15) Uani d . 1
H H27 0.8156 0.6020 0.9418 0.068 Uiso calc R 1
C C28 0.8081(4) 0.5232(4) 0.8309(4) 0.0547(14) Uani d . 1
H H28 0.7764 0.5704 0.7882 0.066 Uiso calc R 1
C C29 0.8303(3) 0.4316(3) 0.7986(4) 0.0452(11) Uani d . 1
C C30 0.8798(3) 0.3602(3) 0.8629(3) 0.0361(10) Uani d . 1
C C31 0.8017(4) 0.4072(4) 0.7045(4) 0.0551(14) Uani d . 1
H H31 0.7696 0.4526 0.6600 0.066 Uiso calc R 1
C C32 0.8213(4) 0.3157(5) 0.6782(4) 0.0598(15) Uani d . 1
H H32 0.8018 0.2980 0.6160 0.072 Uiso calc R 1
C C33 0.8708(4) 0.2504(4) 0.7466(3) 0.0480(12) Uani d . 1
H H33 0.8836 0.1887 0.7281 0.058 Uiso calc R 1
F F1 1.3151(4) 0.3046(6) 0.9873(4) 0.153(3) Uani d . 1
F F2 1.4208(3) 0.3002(4) 0.7394(4) 0.133(2) Uani d . 1
F F3 0.8319(2) -0.2247(2) 0.71639(19) 0.0520(7) Uani d . 1
F F4 0.8467(4) -0.0971(4) 0.4386(2) 0.1107(16) Uani d . 1
F F5 0.6472(2) 0.1067(3) 0.9116(2) 0.0688(9) Uani d . 1
F F6 0.5496(4) 0.0443(4) 1.1648(4) 0.141(2) Uani d . 1
N N1 0.9615(2) 0.3134(3) 1.0209(2) 0.0331(8) Uani d . 1
N N2 0.9010(3) 0.2706(3) 0.8367(2) 0.0355(8) Uani d . 1
O O1 1.1385(2) 0.2404(3) 0.9662(2) 0.0486(8) Uani d . 1
O O2 1.0671(2) 0.1674(2) 0.8334(2) 0.0418(7) Uani d . 1
O O3 0.9197(2) 0.0335(2) 0.84238(19) 0.0360(7) Uani d . 1
O O4 0.9422(2) -0.1250(2) 0.8774(2) 0.0398(7) Uani d . 1
O O5 0.8436(2) 0.1391(2) 0.9743(2) 0.0440(8) Uani d . 1
O O6 0.8994(2) -0.0069(2) 1.0241(2) 0.0449(8) 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'
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'
F F 0.0171 0.0103 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O3 Gd1 O4 . 3_757 130.13(10)
O3 Gd1 O6 . 3_757 73.87(11)
O4 Gd1 O6 3_757 3_757 77.68(10)
O3 Gd1 O5 . . 78.14(11)
O4 Gd1 O5 3_757 . 85.99(12)
O6 Gd1 O5 3_757 . 124.91(11)
O3 Gd1 O1 . . 126.62(10)
O4 Gd1 O1 3_757 . 89.20(11)
O6 Gd1 O1 3_757 . 83.97(12)
O5 Gd1 O1 . . 148.60(11)
O3 Gd1 O2 . . 74.75(10)
O4 Gd1 O2 3_757 . 135.54(11)
O6 Gd1 O2 3_757 . 76.31(11)
O5 Gd1 O2 . . 138.42(11)
O1 Gd1 O2 . . 52.79(10)
O3 Gd1 N2 . . 82.32(11)
O4 Gd1 N2 3_757 . 138.85(11)
O6 Gd1 N2 3_757 . 142.42(11)
O5 Gd1 N2 . . 76.13(11)
O1 Gd1 N2 . . 87.58(12)
O2 Gd1 N2 . . 69.53(11)
O3 Gd1 N1 . . 137.20(11)
O4 Gd1 N1 3_757 . 76.43(11)
O6 Gd1 N1 3_757 . 148.65(11)
O5 Gd1 N1 . . 70.40(11)
O1 Gd1 N1 . . 78.31(11)
O2 Gd1 N1 . . 111.36(11)
N2 Gd1 N1 . . 62.75(11)
O3 Gd1 O6 . . 67.18(9)
O4 Gd1 O6 3_757 . 67.33(10)
O6 Gd1 O6 3_757 . 77.87(11)
O5 Gd1 O6 . . 47.51(10)
O1 Gd1 O6 . . 152.79(11)
O2 Gd1 O6 . . 138.53(10)
N2 Gd1 O6 . . 119.04(10)
N1 Gd1 O6 . . 107.62(10)
O2 C1 O1 . . 121.1(4)
O2 C1 C2 . . 117.8(4)
O1 C1 C2 . . 121.1(4)
C7 C2 C3 . . 116.7(5)
C7 C2 C1 . . 124.1(4)
C3 C2 C1 . . 119.1(4)
C4 C3 C2 . . 120.9(5)
C4 C3 H3 . . 119.6
C2 C3 H3 . . 119.6
C5 C4 C3 . . 119.0(5)
C5 C4 H4 . . 120.5
C3 C4 H4 . . 120.5
C6 C5 C4 . . 122.6(6)
C6 C5 F2 . . 118.5(6)
C4 C5 F2 . . 118.9(6)
C5 C6 C7 . . 119.4(6)
C5 C6 H6 . . 120.3
C7 C6 H6 . . 120.3
F1 C7 C2 . . 122.5(5)
F1 C7 C6 . . 116.0(6)
C2 C7 C6 . . 121.4(5)
O4 C8 O3 . . 126.0(4)
O4 C8 C9 . . 119.7(4)
O3 C8 C9 . . 114.2(4)
C14 C9 C10 . . 117.2(4)
C14 C9 C8 . . 123.9(4)
C10 C9 C8 . . 118.7(4)
C11 C10 C9 . . 121.5(5)
C11 C10 H10 . . 119.3
C9 C10 H10 . . 119.3
C12 C11 C10 . . 118.3(5)
C12 C11 H11 . . 120.8
C10 C11 H11 . . 120.8
C11 C12 C13 . . 123.7(5)
C11 C12 F4 . . 118.3(6)
C13 C12 F4 . . 118.1(6)
C12 C13 C14 . . 116.8(5)
C12 C13 H13 . . 121.6
C14 C13 H13 . . 121.6
F3 C14 C13 . . 117.3(4)
F3 C14 C9 . . 120.3(4)
C13 C14 C9 . . 122.4(5)
O5 C15 O6 . . 123.2(4)
O5 C15 C16 . . 117.4(4)
O6 C15 C16 . . 119.3(4)
C21 C16 C17 . . 117.4(5)
C21 C16 C15 . . 122.3(4)
C17 C16 C15 . . 119.9(5)
C16 C17 C18 . . 120.6(6)
C16 C17 H17 . . 119.7
C18 C17 H17 . . 119.7
C19 C18 C17 . . 119.5(6)
C19 C18 H18 . . 120.3
C17 C18 H18 . . 120.3
C18 C19 F6 . . 120.7(7)
C18 C19 C20 . . 122.7(6)
F6 C19 C20 . . 116.5(8)
C19 C20 C21 . . 117.4(6)
C19 C20 H20 . . 121.3
C21 C20 H20 . . 121.3
F5 C21 C20 . . 117.7(5)
F5 C21 C16 . . 119.9(5)
C20 C21 C16 . . 122.4(6)
N1 C22 C23 . . 123.1(5)
N1 C22 H22 . . 118.4
C23 C22 H22 . . 118.4
C24 C23 C22 . . 119.8(5)
C24 C23 H23 . . 120.1
C22 C23 H23 . . 120.1
C23 C24 C25 . . 119.9(5)
C23 C24 H24 . . 120.1
C25 C24 H24 . . 120.1
C24 C25 C26 . . 116.9(5)
C24 C25 C27 . . 123.2(5)
C26 C25 C27 . . 119.8(5)
N1 C26 C25 . . 123.1(4)
N1 C26 C30 . . 118.1(4)
C25 C26 C30 . . 118.8(4)
C28 C27 C25 . . 121.0(5)
C28 C27 H27 . . 119.5
C25 C27 H27 . . 119.5
C27 C28 C29 . . 121.0(5)
C27 C28 H28 . . 119.5
C29 C28 H28 . . 119.5
C31 C29 C30 . . 117.6(5)
C31 C29 C28 . . 122.5(5)
C30 C29 C28 . . 119.9(5)
N2 C30 C29 . . 122.7(4)
N2 C30 C26 . . 117.8(4)
C29 C30 C26 . . 119.4(4)
C32 C31 C29 . . 119.7(5)
C32 C31 H31 . . 120.2
C29 C31 H31 . . 120.2
C31 C32 C33 . . 118.6(5)
C31 C32 H32 . . 120.7
C33 C32 H32 . . 120.7
N2 C33 C32 . . 124.1(5)
N2 C33 H33 . . 117.9
C32 C33 H33 . . 117.9
C22 N1 C26 . . 117.1(4)
C22 N1 Gd1 . . 122.8(3)
C26 N1 Gd1 . . 119.9(3)
C33 N2 C30 . . 117.3(4)
C33 N2 Gd1 . . 121.4(3)
C30 N2 Gd1 . . 121.3(3)
C1 O1 Gd1 . . 93.1(3)
C1 O2 Gd1 . . 92.7(3)
C8 O3 Gd1 . . 139.2(3)
C8 O4 Gd1 . 3_757 136.2(3)
C15 O5 Gd1 . . 106.2(3)
C15 O6 Gd1 . 3_757 174.2(3)
C15 O6 Gd1 . . 82.5(3)
Gd1 O6 Gd1 3_757 . 102.13(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Gd1 O3 . 2.332(3)
Gd1 O4 3_757 2.391(3)
Gd1 O6 3_757 2.397(3)
Gd1 O5 . 2.429(3)
Gd1 O1 . 2.465(3)
Gd1 O2 . 2.479(3)
Gd1 N2 . 2.597(4)
Gd1 N1 . 2.627(3)
Gd1 O6 . 2.921(4)
C1 O2 . 1.257(5)
C1 O1 . 1.267(5)
C1 C2 . 1.499(6)
C2 C7 . 1.376(7)
C2 C3 . 1.398(7)
C3 C4 . 1.385(7)
C3 H3 . 0.930
C4 C5 . 1.342(9)
C4 H4 . 0.930
C5 C6 . 1.325(10)
C5 F2 . 1.355(6)
C6 C7 . 1.383(9)
C6 H6 . 0.930
C7 F1 . 1.295(7)
C8 O4 . 1.246(5)
C8 O3 . 1.256(5)
C8 C9 . 1.507(5)
C9 C14 . 1.390(6)
C9 C10 . 1.391(6)
C10 C11 . 1.376(6)
C10 H10 . 0.930
C11 C12 . 1.360(8)
C11 H11 . 0.930
C12 C13 . 1.364(9)
C12 F4 . 1.364(6)
C13 C14 . 1.387(7)
C13 H13 . 0.930
C14 F3 . 1.335(6)
C15 O5 . 1.247(5)
C15 O6 . 1.255(5)
C15 C16 . 1.509(6)
C16 C21 . 1.382(7)
C16 C17 . 1.388(7)
C17 C18 . 1.391(9)
C17 H17 . 0.930
C18 C19 . 1.334(11)
C18 H18 . 0.930
C19 F6 . 1.359(7)
C19 C20 . 1.372(10)
C20 C21 . 1.381(8)
C20 H20 . 0.930
C21 F5 . 1.346(6)
C22 N1 . 1.334(6)
C22 C23 . 1.395(7)
C22 H22 . 0.930
C23 C24 . 1.353(8)
C23 H23 . 0.930
C24 C25 . 1.402(7)
C24 H24 . 0.930
C25 C26 . 1.416(6)
C25 C27 . 1.431(7)
C26 N1 . 1.362(6)
C26 C30 . 1.444(7)
C27 C28 . 1.348(8)
C27 H27 . 0.930
C28 C29 . 1.426(7)
C28 H28 . 0.930
C29 C31 . 1.398(8)
C29 C30 . 1.411(6)
C30 N2 . 1.358(5)
C31 C32 . 1.375(8)
C31 H31 . 0.930
C32 C33 . 1.390(7)
C32 H32 . 0.930
C33 N2 . 1.329(6)
C33 H33 . 0.930
O4 Gd1 3_757 2.391(3)
O6 Gd1 3_757 2.397(3)
