#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:08:31 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229787 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/53/7045310.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_7045310
loop_
_publ_author_name
'García-Rodríguez, Raúl'
'Kopf, Sara'
'Wright, Dominic S.'
_publ_section_title
;
 Modifying the donor properties of tris(pyridyl)aluminates in
 lanthanide(ii) sandwich compounds.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2232
_journal_page_last               2239
_journal_paper_doi               10.1039/c7dt04657j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C40 H46 Al2 Eu N6'
_chemical_formula_sum            'C40 H46 Al2 Eu N6'
_chemical_formula_weight         816.75
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-11-24 deposited with the CCDC.
2018-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5238(2)
_cell_length_b                   10.5238(2)
_cell_length_c                   35.4237(7)
_cell_measurement_reflns_used    5757
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      66.45
_cell_measurement_theta_min      4.38
_cell_volume                     3923.19(13)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            21577
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.767
_diffrn_reflns_theta_max         66.767
_diffrn_reflns_theta_min         4.383
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    12.144
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_correction_T_min  0.370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/hexane'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Flack x determined using 871 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0225P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0756
_reflns_Friedel_coverage         0.647
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                2780
_reflns_number_total             3464
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt04657j2.cif
_cod_data_source_block           compound_3
_cod_depositor_comments
'Adding full bibliography for 7045310--7045315.cif.'
_cod_original_cell_volume        3923.19(17)
_cod_database_code               7045310
_shelx_shelxl_version_number     2014/7
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+3/4'
'y+1/2, -x+1/2, z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'x+1/2, -y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -z+1/2'
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
_atom_site_refinement_flags_occupancy
Eu1 Eu 0.70806(4) 0.29194(4) 0.2500 0.03366(17) Uani 1 2 d S T P
Al1 Al 0.95157(17) 0.52405(17) 0.23823(5) 0.0336(5) Uani 1 1 d . . .
N2 N 0.9284(5) 0.2482(5) 0.21474(14) 0.0327(13) Uani 1 1 d . . .
N1 N 0.8296(6) 0.4172(5) 0.30638(15) 0.0528(17) Uani 1 1 d . . .
C22 C 1.1384(6) 0.3268(6) 0.22162(17) 0.0398(18) Uani 1 1 d . . .
H22 H 1.1942 0.3944 0.2280 0.048 Uiso 1 1 calc R U .
C21 C 1.0068(6) 0.3482(6) 0.22318(16) 0.0303(15) Uani 1 1 d . . .
C25 C 0.9770(7) 0.1351(7) 0.20408(17) 0.0388(17) Uani 1 1 d . . .
C31 C 0.7895(7) 0.5774(6) 0.21182(17) 0.0379(16) Uani 1 1 d . . .
C23 C 1.1898(7) 0.2113(8) 0.21118(16) 0.0491(17) Uani 1 1 d . . .
H23 H 1.2791 0.1983 0.2105 0.059 Uiso 1 1 calc R U .
C24 C 1.1067(7) 0.1162(7) 0.20181(18) 0.0467(18) Uani 1 1 d . . .
H24 H 1.1387 0.0363 0.1937 0.056 Uiso 1 1 calc R U .
C32 C 0.7888(7) 0.6900(6) 0.19166(17) 0.0426(16) Uani 1 1 d . . .
H32 H 0.8650 0.7380 0.1898 0.051 Uiso 1 1 calc R U .
C11 C 0.9213(7) 0.5023(6) 0.29389(17) 0.0403(17) Uani 1 1 d . . .
C33 C 0.6811(7) 0.7346(6) 0.1742(2) 0.055(2) Uani 1 1 d . . .
H33 H 0.6832 0.8128 0.1608 0.065 Uiso 1 1 calc R U .
C12 C 0.9946(7) 0.5656(7) 0.32101(18) 0.0445(17) Uani 1 1 d . . .
H12 H 1.0582 0.6237 0.3130 0.053 Uiso 1 1 calc R U .
N3 N 0.6792(6) 0.5102(6) 0.2134(2) 0.071(2) Uani 1 1 d . . .
C13 C 0.9761(8) 0.5453(8) 0.35927(19) 0.057(2) Uani 1 1 d . . .
H13 H 1.0262 0.5883 0.3775 0.069 Uiso 1 1 calc R U .
C15 C 0.8143(9) 0.3984(7) 0.3437(2) 0.065(2) Uani 1 1 d . . .
C14 C 0.8835(10) 0.4616(8) 0.3700(2) 0.070(2) Uani 1 1 d . . .
H14 H 0.8676 0.4475 0.3960 0.083 Uiso 1 1 calc R U .
C1 C 1.0885(7) 0.6522(7) 0.22977(19) 0.0499(19) Uani 1 1 d . . .
H1A H 1.0567 0.7354 0.2388 0.060 Uiso 1 1 calc R U .
H1B H 1.1614 0.6289 0.2460 0.060 Uiso 1 1 calc R U .
C26 C 0.8846(8) 0.0321(7) 0.1940(2) 0.064(2) Uani 1 1 d . . .
H26A H 0.8267 0.0175 0.2152 0.096 Uiso 1 1 calc R U .
H26B H 0.9312 -0.0464 0.1884 0.096 Uiso 1 1 calc R U .
H26C H 0.8357 0.0577 0.1717 0.096 Uiso 1 1 calc R U .
C34 C 0.5725(7) 0.6673(8) 0.1761(3) 0.080(3) Uani 1 1 d . . .
H34 H 0.4973 0.6963 0.1640 0.096 Uiso 1 1 calc R U .
C2 C 1.1387(7) 0.6705(7) 0.1894(2) 0.065(2) Uani 1 1 d . . .
H2A H 1.1683 0.5888 0.1795 0.097 Uiso 1 1 calc R U .
H2B H 1.2095 0.7310 0.1897 0.097 Uiso 1 1 calc R U .
H2C H 1.0705 0.7034 0.1734 0.097 Uiso 1 1 calc R U .
C16 C 0.7147(11) 0.3025(9) 0.3559(2) 0.121(4) Uani 1 1 d . . .
H16A H 0.6328 0.3454 0.3590 0.182 Uiso 1 1 calc R U .
H16B H 0.7402 0.2640 0.3799 0.182 Uiso 1 1 calc R U .
H16C H 0.7070 0.2361 0.3366 0.182 Uiso 1 1 calc R U .
C35 C 0.5739(8) 0.5549(9) 0.1961(3) 0.098(4) Uani 1 1 d . . .
C36 C 0.4530(10) 0.4759(12) 0.1981(5) 0.208(9) Uani 1 1 d . . .
H36A H 0.4745 0.3855 0.1962 0.313 Uiso 1 1 calc R U .
H36B H 0.3965 0.4995 0.1773 0.313 Uiso 1 1 calc R U .
H36C H 0.4101 0.4918 0.2222 0.313 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -8.9294 11.1857 '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
N3 Eu1 N3 92.3(3) . 8_665
N3 Eu1 N2 91.13(16) . .
N3 Eu1 N2 176.46(18) 8_665 .
N3 Eu1 N2 176.46(18) . 8_665
N3 Eu1 N2 91.13(16) 8_665 8_665
N2 Eu1 N2 85.4(2) . 8_665
N3 Eu1 N1 89.61(19) . .
N3 Eu1 N1 89.6(2) 8_665 .
N2 Eu1 N1 91.07(16) . .
N2 Eu1 N1 89.79(17) 8_665 .
N3 Eu1 N1 89.6(2) . 8_665
N3 Eu1 N1 89.62(19) 8_665 8_665
N2 Eu1 N1 89.79(17) . 8_665
N2 Eu1 N1 91.07(16) 8_665 8_665
N1 Eu1 N1 178.8(3) . 8_665
N3 Eu1 Al1 55.41(14) . .
N3 Eu1 Al1 126.91(14) 8_665 .
N2 Eu1 Al1 55.93(11) . .
N2 Eu1 Al1 121.68(11) 8_665 .
N1 Eu1 Al1 54.14(12) . .
N1 Eu1 Al1 125.89(12) 8_665 .
N3 Eu1 Al1 126.91(14) . 8_665
N3 Eu1 Al1 55.42(14) 8_665 8_665
N2 Eu1 Al1 121.68(11) . 8_665
N2 Eu1 Al1 55.94(11) 8_665 8_665
N1 Eu1 Al1 125.89(12) . 8_665
N1 Eu1 Al1 54.14(12) 8_665 8_665
Al1 Eu1 Al1 177.27(6) . 8_665
C1 Al1 C21 111.9(3) . .
C1 Al1 C11 109.8(3) . .
C21 Al1 C11 101.6(2) . .
C1 Al1 C31 110.6(3) . .
C21 Al1 C31 112.1(3) . .
C11 Al1 C31 110.6(3) . .
C1 Al1 Eu1 178.0(2) . .
C21 Al1 Eu1 66.95(18) . .
C11 Al1 Eu1 72.1(2) . .
C31 Al1 Eu1 68.80(18) . .
C25 N2 C21 120.7(5) . .
C25 N2 Eu1 127.7(4) . .
C21 N2 Eu1 106.8(4) . .
C15 N1 C11 119.4(6) . .
C15 N1 Eu1 126.5(5) . .
C11 N1 Eu1 114.0(4) . .
C23 C22 C21 122.5(6) . .
C23 C22 H22 118.7 . .
C21 C22 H22 118.7 . .
N2 C21 C22 117.5(6) . .
N2 C21 Al1 126.2(4) . .
C22 C21 Al1 116.3(5) . .
N2 C25 C24 121.2(7) . .
N2 C25 C26 117.3(7) . .
C24 C25 C26 121.5(7) . .
N3 C31 C32 117.5(6) . .
N3 C31 Al1 123.8(4) . .
C32 C31 Al1 118.7(5) . .
C24 C23 C22 117.3(7) . .
C24 C23 H23 121.4 . .
C22 C23 H23 121.4 . .
C23 C24 C25 120.8(7) . .
C23 C24 H24 119.6 . .
C25 C24 H24 119.6 . .
C33 C32 C31 121.9(7) . .
C33 C32 H32 119.0 . .
C31 C32 H32 119.0 . .
N1 C11 C12 118.1(6) . .
N1 C11 Al1 119.7(5) . .
C12 C11 Al1 122.1(5) . .
C34 C33 C32 119.9(6) . .
C34 C33 H33 120.0 . .
C32 C33 H33 120.0 . .
C13 C12 C11 121.3(7) . .
C13 C12 H12 119.3 . .
C11 C12 H12 119.3 . .
C35 N3 C31 120.0(6) . .
C35 N3 Eu1 128.1(5) . .
C31 N3 Eu1 111.8(4) . .
C14 C13 C12 118.1(7) . .
C14 C13 H13 121.0 . .
C12 C13 H13 121.0 . .
N1 C15 C14 122.5(7) . .
N1 C15 C16 117.4(7) . .
C14 C15 C16 120.1(7) . .
C15 C14 C13 120.6(7) . .
C15 C14 H14 119.7 . .
C13 C14 H14 119.7 . .
C2 C1 Al1 118.2(5) . .
C2 C1 H1A 107.8 . .
Al1 C1 H1A 107.8 . .
C2 C1 H1B 107.8 . .
Al1 C1 H1B 107.8 . .
H1A C1 H1B 107.1 . .
C25 C26 H26A 109.5 . .
C25 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C25 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
C33 C34 C35 117.9(7) . .
C33 C34 H34 121.1 . .
C35 C34 H34 121.1 . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
N3 C35 C34 122.7(7) . .
N3 C35 C36 118.3(8) . .
C34 C35 C36 118.9(8) . .
C35 C36 H36A 109.5 . .
C35 C36 H36B 109.5 . .
H36A C36 H36B 109.5 . .
C35 C36 H36C 109.5 . .
H36A C36 H36C 109.5 . .
H36B C36 H36C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Eu1 N3 2.655(6) .
Eu1 N3 2.655(6) 8_665
Eu1 N2 2.674(5) .
Eu1 N2 2.674(5) 8_665
Eu1 N1 2.713(6) .
Eu1 N1 2.713(6) 8_665
Eu1 Al1 3.5648(18) .
Eu1 Al1 3.5648(18) 8_665
Al1 C1 1.996(6) .
Al1 C21 2.012(6) .
Al1 C11 2.010(6) .
Al1 C31 2.025(7) .
N2 C25 1.350(8) .
N2 C21 1.370(7) .
N1 C15 1.346(8) .
N1 C11 1.389(9) .
C22 C23 1.381(9) .
C22 C21 1.404(8) .
C22 H22 0.9500 .
C25 C24 1.382(9) .
C25 C26 1.499(9) .
C31 N3 1.360(8) .
C31 C32 1.384(8) .
C23 C24 1.369(9) .
C23 H23 0.9500 .
C24 H24 0.9500 .
C32 C33 1.374(8) .
C32 H32 0.9500 .
C11 C12 1.401(9) .
C33 C34 1.346(10) .
C33 H33 0.9500 .
C12 C13 1.386(9) .
C12 H12 0.9500 .
N3 C35 1.350(9) .
C13 C14 1.367(10) .
C13 H13 0.9500 .
C15 C14 1.356(10) .
C15 C16 1.518(11) .
C14 H14 0.9500 .
C1 C2 1.535(9) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
C34 C35 1.379(10) .
C34 H34 0.9500 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C35 C36 1.522(11) .
C36 H36A 0.9800 .
C36 H36B 0.9800 .
C36 H36C 0.9800 .
