#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:08:31 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229787 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/53/7045313.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_7045313
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         'C34 H28 Al2 Br6 Eu N6,2(C4 H8 O)'
_chemical_formula_sum            'C42 H44 Al2 Br6 Eu N6 O2'
_chemical_formula_weight         1350.21
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                92.2140(10)
_cell_angle_beta                 113.3580(10)
_cell_angle_gamma                108.4810(10)
_cell_formula_units_Z            1
_cell_length_a                   10.8508(2)
_cell_length_b                   10.9222(2)
_cell_length_c                   11.6496(3)
_cell_measurement_reflns_used    7553
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1180.53(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12740
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.518
_diffrn_reflns_theta_min         2.683
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.484
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_description       block
_exptl_crystal_F_000             653
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/hexane'
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.497
_refine_diff_density_min         -1.453
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         5257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²+0.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4181
_reflns_number_total             5257
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt04657j2.cif
_cod_data_source_block           compound_6
_cod_depositor_comments
'Adding full bibliography for 7045310--7045315.cif.'
_cod_original_cell_volume        1180.53(4)
_cod_database_code               7045313
_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.
;
_shelx_estimated_absorpt_t_min   0.464
_shelx_estimated_absorpt_t_max   0.738
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
_atom_site_refinement_flags_occupancy
Eu01 Eu 0.500000 0.500000 0.500000 0.02529(13) Uani 1 2 d S . P
Br2 Br 0.24455(7) 0.17373(6) 0.51009(6) 0.04151(18) Uani 1 1 d . . .
Br3 Br 0.65437(7) 0.50517(7) 0.26079(6) 0.04149(18) Uani 1 1 d . . .
Br1 Br 0.70784(7) 0.75007(6) 0.79974(6) 0.04357(19) Uani 1 1 d . . .
Al1 Al 0.22122(16) 0.65080(14) 0.32762(15) 0.0234(3) Uani 1 1 d . . .
N3 N 0.4397(5) 0.5837(4) 0.2706(4) 0.0255(9) Uani 1 1 d . . .
N2 N 0.2057(5) 0.3948(4) 0.4173(4) 0.0248(9) Uani 1 1 d . . .
N1 N 0.4731(5) 0.7310(4) 0.5796(4) 0.0261(9) Uani 1 1 d . . .
O1T O 0.2552(6) 0.9198(5) 0.9507(6) 0.0603(14) Uani 1 1 d . . .
C31 C 0.3348(6) 0.6374(5) 0.2302(5) 0.0258(10) Uani 1 1 d . . .
C12 C 0.3597(6) 0.8892(5) 0.5343(6) 0.0307(12) Uani 1 1 d . . .
H12 H 0.286922 0.916898 0.477822 0.037 Uiso 1 1 calc R U .
C32 C 0.3104(6) 0.6896(5) 0.1180(5) 0.0304(12) Uani 1 1 d . . .
H32 H 0.239164 0.728366 0.089915 0.036 Uiso 1 1 calc R U .
C23 C -0.0784(7) 0.3234(6) 0.3811(7) 0.0412(15) Uani 1 1 d . . .
H23 H -0.174947 0.301478 0.369969 0.049 Uiso 1 1 calc R U .
C34 C 0.4904(6) 0.6299(5) 0.0895(5) 0.0308(12) Uani 1 1 d . . .
H34 H 0.545347 0.625098 0.044306 0.037 Uiso 1 1 calc R U .
C11 C 0.3654(5) 0.7682(5) 0.4972(5) 0.0252(10) Uani 1 1 d . . .
C24 C -0.0024(6) 0.2424(5) 0.4303(6) 0.0352(13) Uani 1 1 d . . .
H24 H -0.044476 0.162756 0.453534 0.042 Uiso 1 1 calc R U .
C13 C 0.4568(7) 0.9689(5) 0.6504(6) 0.0363(13) Uani 1 1 d . . .
H13 H 0.451175 1.050637 0.673476 0.044 Uiso 1 1 calc R U .
C1 C 0.0702(6) 0.7234(6) 0.2338(6) 0.0343(13) Uani 1 1 d . . .
H1A H 0.024522 0.736631 0.289439 0.041 Uiso 1 1 calc R U .
H1B H 0.118531 0.811052 0.219762 0.041 Uiso 1 1 calc R U .
C14 C 0.5625(7) 0.9288(5) 0.7332(6) 0.0367(13) Uani 1 1 d . . .
H14 H 0.629999 0.979954 0.814971 0.044 Uiso 1 1 calc R U .
C21 C 0.1326(6) 0.4754(5) 0.3677(5) 0.0265(11) Uani 1 1 d . . .
C22 C -0.0106(6) 0.4359(5) 0.3488(7) 0.0388(14) Uani 1 1 d . . .
H22 H -0.063749 0.489720 0.311733 0.047 Uiso 1 1 calc R U .
C2 C -0.0480(7) 0.6425(7) 0.1064(6) 0.0458(15) Uani 1 1 d . . .
H2A H -0.006403 0.637037 0.046378 0.069 Uiso 1 1 calc R U .
H2B H -0.119540 0.684252 0.073054 0.069 Uiso 1 1 calc R U .
H2C H -0.094612 0.553776 0.117371 0.069 Uiso 1 1 calc R U .
C33 C 0.3858(7) 0.6866(5) 0.0472(6) 0.0360(13) Uani 1 1 d . . .
H33 H 0.366997 0.722279 -0.028329 0.043 Uiso 1 1 calc R U .
C35 C 0.5103(6) 0.5810(5) 0.2006(5) 0.0272(11) Uani 1 1 d . . .
C15 C 0.5641(6) 0.8094(5) 0.6898(5) 0.0301(11) Uani 1 1 d . . .
C4T C 0.1061(8) 0.8905(7) 0.9108(7) 0.0468(15) Uani 1 1 d . . .
H4T1 H 0.081942 0.880588 0.984245 0.056 Uiso 1 1 calc R U .
H4T2 H 0.049480 0.807651 0.847218 0.056 Uiso 1 1 calc R U .
C25 C 0.1364(6) 0.2830(5) 0.4438(5) 0.0291(11) Uani 1 1 d . . .
C3T C 0.0728(8) 1.0031(6) 0.8531(8) 0.0551(18) Uani 1 1 d . . .
H3T1 H -0.019804 0.971010 0.775638 0.066 Uiso 1 1 calc R U .
H3T2 H 0.067347 1.063965 0.914508 0.066 Uiso 1 1 calc R U .
C2T C 0.1944(10) 1.0696(8) 0.8209(10) 0.077(3) Uani 1 1 d . . .
H2T1 H 0.166519 1.043377 0.729189 0.093 Uiso 1 1 calc R U .
H2T2 H 0.224828 1.166288 0.841899 0.093 Uiso 1 1 calc R U .
C1T C 0.3111(11) 1.0254(11) 0.8993(12) 0.094(4) Uani 1 1 d . . .
H1T1 H 0.353427 0.997956 0.846332 0.112 Uiso 1 1 calc R U .
H1T2 H 0.387917 1.098502 0.968740 0.112 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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N3 Eu01 N3 180.0 2_666 .
N3 Eu01 N2 94.40(12) 2_666 .
N3 Eu01 N2 85.60(12) . .
N3 Eu01 N2 85.60(12) 2_666 2_666
N3 Eu01 N2 94.40(12) . 2_666
N2 Eu01 N2 180.0 . 2_666
N3 Eu01 N1 95.88(12) 2_666 .
N3 Eu01 N1 84.12(12) . .
N2 Eu01 N1 84.16(12) . .
N2 Eu01 N1 95.84(12) 2_666 .
N3 Eu01 N1 84.12(12) 2_666 2_666
N3 Eu01 N1 95.88(12) . 2_666
N2 Eu01 N1 95.84(12) . 2_666
N2 Eu01 N1 84.16(12) 2_666 2_666
N1 Eu01 N1 180.0 . 2_666
C1 Al1 C31 111.3(2) . .
C1 Al1 C21 110.6(2) . .
C31 Al1 C21 111.3(2) . .
C1 Al1 C11 111.5(2) . .
C31 Al1 C11 106.1(2) . .
C21 Al1 C11 105.8(2) . .
C35 N3 C31 118.4(4) . .
C35 N3 Eu01 124.1(3) . .
C31 N3 Eu01 117.4(3) . .
C25 N2 C21 118.4(4) . .
C25 N2 Eu01 124.2(3) . .
C21 N2 Eu01 116.1(3) . .
C15 N1 C11 118.6(4) . .
C15 N1 Eu01 122.6(3) . .
C11 N1 Eu01 118.7(3) . .
C1T O1T C4T 110.0(6) . .
N3 C31 C32 118.0(4) . .
N3 C31 Al1 122.9(4) . .
C32 C31 Al1 119.1(4) . .
C13 C12 C11 121.7(5) . .
C13 C12 H12 119.2 . .
C11 C12 H12 119.2 . .
C33 C32 C31 122.6(5) . .
C33 C32 H32 118.7 . .
C31 C32 H32 118.7 . .
C22 C23 C24 118.2(5) . .
C22 C23 H23 120.9 . .
C24 C23 H23 120.9 . .
C35 C34 C33 116.7(5) . .
C35 C34 H34 121.6 . .
C33 C34 H34 121.6 . .
N1 C11 C12 118.2(5) . .
N1 C11 Al1 120.3(4) . .
C12 C11 Al1 121.5(4) . .
C25 C24 C23 116.6(5) . .
C25 C24 H24 121.7 . .
C23 C24 H24 121.7 . .
C12 C13 C14 119.4(5) . .
C12 C13 H13 120.3 . .
C14 C13 H13 120.3 . .
C2 C1 Al1 117.0(4) . .
C2 C1 H1A 108.0 . .
Al1 C1 H1A 108.0 . .
C2 C1 H1B 108.0 . .
Al1 C1 H1B 108.0 . .
H1A C1 H1B 107.3 . .
C13 C14 C15 116.1(6) . .
C13 C14 H14 122.0 . .
C15 C14 H14 122.0 . .
N2 C21 C22 117.5(5) . .
N2 C21 Al1 124.0(4) . .
C22 C21 Al1 118.4(4) . .
C23 C22 C21 123.3(5) . .
C23 C22 H22 118.3 . .
C21 C22 H22 118.3 . .
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 . .
C32 C33 C34 118.2(5) . .
C32 C33 H33 120.9 . .
C34 C33 H33 120.9 . .
N3 C35 C34 126.1(5) . .
N3 C35 Br3 116.7(4) . .
C34 C35 Br3 117.2(4) . .
N1 C15 C14 126.0(5) . .
N1 C15 Br1 116.2(4) . .
C14 C15 Br1 117.8(4) . .
O1T C4T C3T 106.8(5) . .
O1T C4T H4T1 110.4 . .
C3T C4T H4T1 110.4 . .
O1T C4T H4T2 110.4 . .
C3T C4T H4T2 110.4 . .
H4T1 C4T H4T2 108.6 . .
N2 C25 C24 125.9(5) . .
N2 C25 Br2 116.1(4) . .
C24 C25 Br2 117.9(4) . .
C2T C3T C4T 104.9(6) . .
C2T C3T H3T1 110.8 . .
C4T C3T H3T1 110.8 . .
C2T C3T H3T2 110.8 . .
C4T C3T H3T2 110.8 . .
H3T1 C3T H3T2 108.9 . .
C1T C2T C3T 105.0(6) . .
C1T C2T H2T1 110.8 . .
C3T C2T H2T1 110.8 . .
C1T C2T H2T2 110.8 . .
C3T C2T H2T2 110.8 . .
H2T1 C2T H2T2 108.8 . .
O1T C1T C2T 109.2(7) . .
O1T C1T H1T1 109.8 . .
C2T C1T H1T1 109.8 . .
O1T C1T H1T2 109.8 . .
C2T C1T H1T2 109.8 . .
H1T1 C1T H1T2 108.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Eu01 N3 2.754(4) 2_666
Eu01 N3 2.754(4) .
Eu01 N2 2.756(4) .
Eu01 N2 2.756(4) 2_666
Eu01 N1 2.795(4) .
Eu01 N1 2.795(4) 2_666
Br2 C25 1.908(5) .
Br3 C35 1.902(5) .
Br1 C15 1.901(6) .
Al1 C1 1.994(5) .
Al1 C31 2.010(5) .
Al1 C21 2.018(5) .
Al1 C11 2.019(6) .
N3 C35 1.328(7) .
N3 C31 1.371(6) .
N2 C25 1.335(7) .
N2 C21 1.363(6) .
N1 C15 1.315(7) .
N1 C11 1.376(7) .
O1T C1T 1.398(9) .
O1T C4T 1.415(8) .
C31 C32 1.409(7) .
C12 C13 1.377(9) .
C12 C11 1.402(7) .
C12 H12 0.9500 .
C32 C33 1.378(8) .
C32 H32 0.9500 .
C23 C22 1.369(8) .
C23 C24 1.385(9) .
C23 H23 0.9500 .
C34 C35 1.383(7) .
C34 C33 1.393(8) .
C34 H34 0.9500 .
C24 C25 1.369(8) .
C24 H24 0.9500 .
C13 C14 1.382(9) .
C13 H13 0.9500 .
C1 C2 1.517(9) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C14 C15 1.389(8) .
C14 H14 0.9500 .
C21 C22 1.395(7) .
C22 H22 0.9500 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C33 H33 0.9500 .
C4T C3T 1.499(9) .
C4T H4T1 0.9900 .
C4T H4T2 0.9900 .
C3T C2T 1.488(11) .
C3T H3T1 0.9900 .
C3T H3T2 0.9900 .
C2T C1T 1.474(13) .
C2T H2T1 0.9900 .
C2T H2T2 0.9900 .
C1T H1T1 0.9900 .
C1T H1T2 0.9900 .
