#------------------------------------------------------------------------------
#$Date: 2021-02-05 01:27:50 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261741 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/01/7060181.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_7060181
loop_
_publ_author_name
'Rösch, Andreas'
'Seifert, Fabian'
'Vass, Valentin'
'Görls, Helmar'
'Kretschmer, Robert'
_publ_section_title
;
 Synthesis, structure, and catalytic activity of dinuclear aluminium
 bis(amidinate) and bis(guanidinate) complexes
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              972
_journal_page_last               981
_journal_paper_doi               10.1039/D0NJ05007E
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C40 H68 Al2 N4'
_chemical_formula_sum            'C40 H68 Al2 N4'
_chemical_formula_weight         658.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-10-09 deposited with the CCDC.	2020-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.849(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1318(2)
_cell_length_b                   13.1042(3)
_cell_length_c                   17.6741(3)
_cell_measurement_reflns_used    11805
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      73.583
_cell_measurement_theta_min      4.245
_cell_volume                     2053.49(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11805
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.583
_diffrn_reflns_theta_min         4.245
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) 
Numerical absorption correction based on gaussian integration over 
   a multifaceted crystal model 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0337
_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)+(0.0504P)²+0.5635P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3693
_reflns_number_total             3998
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0nj05007e2.cif
_cod_data_source_block           FO7074_3a
_cod_depositor_comments
'Adding full bibliography for 7060181--7060191.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7060181
_shelx_shelxl_version_number     2018/3
_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   0.892
_shelx_estimated_absorpt_t_max   0.939
loop_
_space_group_symop_operation_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_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
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.86160(4) 0.37923(2) 0.62013(2) 0.02223(11) Uani 1 1 d . . . . .
N2 N 0.90841(11) 0.50850(7) 0.58118(5) 0.0215(2) Uani 1 1 d . . . . .
N1 N 0.81277(10) 0.49181(7) 0.68141(5) 0.02008(19) Uani 1 1 d . . . . .
C1 C 0.76467(12) 0.50603(8) 0.75153(6) 0.0201(2) Uani 1 1 d . . . . .
C2 C 0.87170(13) 0.50951(8) 0.82359(7) 0.0235(2) Uani 1 1 d . . . . .
C3 C 0.81999(15) 0.51672(9) 0.89140(7) 0.0294(3) Uani 1 1 d . . . . .
H3A H 0.891072 0.519931 0.940340 0.035 Uiso 1 1 calc R U . . .
C4 C 0.66783(16) 0.51933(10) 0.88920(7) 0.0320(3) Uani 1 1 d . . . . .
H4A H 0.634907 0.524599 0.936133 0.038 Uiso 1 1 calc R U . . .
C5 C 0.56365(14) 0.51420(9) 0.81809(7) 0.0287(3) Uani 1 1 d . . . . .
H5A H 0.459060 0.515141 0.816811 0.034 Uiso 1 1 calc R U . . .
C6 C 0.60891(13) 0.50771(8) 0.74846(7) 0.0236(2) Uani 1 1 d . . . . .
C7 C 1.04103(14) 0.50409(9) 0.83018(7) 0.0293(3) Uani 1 1 d . . . . .
H7A H 1.057406 0.505634 0.776236 0.035 Uiso 1 1 calc R U . . .
C8 C 1.10634(16) 0.40355(11) 0.86846(8) 0.0401(3) Uani 1 1 d . . . . .
H8A H 1.056479 0.345993 0.837241 0.060 Uiso 1 1 calc R U . . .
H8B H 1.089368 0.399360 0.921064 0.060 Uiso 1 1 calc R U . . .
H8C H 1.214858 0.401117 0.871515 0.060 Uiso 1 1 calc R U . . .
C9 C 1.12611(15) 0.59478(11) 0.87526(8) 0.0386(3) Uani 1 1 d . . . . .
H9A H 1.083591 0.658661 0.850612 0.058 Uiso 1 1 calc R U . . .
H9B H 1.233011 0.590577 0.874733 0.058 Uiso 1 1 calc R U . . .
H9C H 1.116069 0.593009 0.929219 0.058 Uiso 1 1 calc R U . . .
C10 C 0.49253(13) 0.50019(9) 0.67102(7) 0.0280(3) Uani 1 1 d . . . . .
H10A H 0.543871 0.518194 0.628790 0.034 Uiso 1 1 calc R U . . .
C11 C 0.35858(15) 0.57287(11) 0.66441(9) 0.0413(3) Uani 1 1 d . . . . .
H11A H 0.395815 0.642640 0.676042 0.062 Uiso 1 1 calc R U . . .
H11B H 0.299858 0.552351 0.701592 0.062 Uiso 1 1 calc R U . . .
H11C H 0.294419 0.570083 0.611374 0.062 Uiso 1 1 calc R U . . .
C12 C 0.43747(15) 0.39021(10) 0.65780(8) 0.0373(3) Uani 1 1 d . . . . .
H12A H 0.524253 0.344527 0.662862 0.056 Uiso 1 1 calc R U . . .
H12B H 0.371503 0.383626 0.605416 0.056 Uiso 1 1 calc R U . . .
H12C H 0.381295 0.371837 0.696617 0.056 Uiso 1 1 calc R U . . .
C13 C 0.85712(11) 0.56051(8) 0.63468(6) 0.0190(2) Uani 1 1 d . . . . .
C14 C 0.85135(12) 0.67732(8) 0.63931(6) 0.0211(2) Uani 1 1 d . . . . .
C15 C 0.77189(13) 0.71749(9) 0.70063(7) 0.0265(2) Uani 1 1 d . . . . .
H15A H 0.826636 0.694540 0.752464 0.040 Uiso 1 1 calc R U . . .
H15B H 0.668385 0.691348 0.689410 0.040 Uiso 1 1 calc R U . . .
H15C H 0.769913 0.792250 0.699182 0.040 Uiso 1 1 calc R U . . .
C16 C 0.76372(14) 0.72030(9) 0.56013(7) 0.0295(3) Uani 1 1 d . . . . .
H16A H 0.664815 0.687185 0.544755 0.044 Uiso 1 1 calc R U . . .
H16B H 0.820507 0.706991 0.520618 0.044 Uiso 1 1 calc R U . . .
H16C H 0.750162 0.794043 0.564716 0.044 Uiso 1 1 calc R U . . .
C17 C 1.01368(13) 0.71887(9) 0.65956(7) 0.0272(2) Uani 1 1 d . . . . .
H17A H 1.068283 0.691324 0.709987 0.041 Uiso 1 1 calc R U . . .
H17B H 1.011327 0.793519 0.662432 0.041 Uiso 1 1 calc R U . . .
H17C H 1.064820 0.698233 0.619174 0.041 Uiso 1 1 calc R U . . .
C18 C 0.69402(17) 0.31091(11) 0.54803(8) 0.0414(3) Uani 1 1 d . . . . .
H18A H 0.654720 0.256290 0.575506 0.062 Uiso 1 1 calc R U . . .
H18B H 0.729681 0.281779 0.504605 0.062 Uiso 1 1 calc R U . . .
H18C H 0.613786 0.360465 0.527887 0.062 Uiso 1 1 calc R U . . .
C19 C 1.03441(16) 0.29531(10) 0.66969(8) 0.0371(3) Uani 1 1 d . . . . .
H19A H 1.001923 0.242101 0.701068 0.056 Uiso 1 1 calc R U . . .
H19B H 1.111104 0.338165 0.703354 0.056 Uiso 1 1 calc R U . . .
H19C H 1.077007 0.263500 0.629556 0.056 Uiso 1 1 calc R U . . .
C20 C 0.95771(12) 0.54373(8) 0.51365(6) 0.0204(2) Uani 1 1 d . . . . .
H20A H 1.024710 0.603702 0.527484 0.025 Uiso 1 1 calc R U . . .
H20B H 0.869666 0.563817 0.471696 0.025 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'
Al Al 0.2130 0.2455 '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'
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
_geom_angle_publ_flag
N2 Al1 N1 68.26(4) . . ?
N2 Al1 C19 115.72(5) . . ?
N1 Al1 C19 116.51(5) . . ?
N2 Al1 C18 112.18(6) . . ?
N1 Al1 C18 117.50(6) . . ?
C19 Al1 C18 117.18(7) . . ?
C13 N2 C20 130.58(9) . . ?
C13 N2 Al1 92.90(7) . . ?
C20 N2 Al1 135.92(7) . . ?
C13 N1 C1 130.32(9) . . ?
C13 N1 Al1 91.31(7) . . ?
C1 N1 Al1 138.12(7) . . ?
C2 C1 C6 120.62(10) . . ?
C2 C1 N1 119.99(10) . . ?
C6 C1 N1 119.17(10) . . ?
C3 C2 C1 118.40(11) . . ?
C3 C2 C7 118.96(10) . . ?
C1 C2 C7 122.64(10) . . ?
C4 C3 C2 121.57(11) . . ?
C4 C3 H3A 119.2 . . ?
C2 C3 H3A 119.2 . . ?
C3 C4 C5 119.50(11) . . ?
C3 C4 H4A 120.3 . . ?
C5 C4 H4A 120.3 . . ?
C4 C5 C6 121.39(11) . . ?
C4 C5 H5A 119.3 . . ?
C6 C5 H5A 119.3 . . ?
C5 C6 C1 118.51(10) . . ?
C5 C6 C10 120.54(11) . . ?
C1 C6 C10 120.94(10) . . ?
C2 C7 C9 112.45(11) . . ?
C2 C7 C8 110.71(11) . . ?
C9 C7 C8 109.93(11) . . ?
C2 C7 H7A 107.9 . . ?
C9 C7 H7A 107.9 . . ?
C8 C7 H7A 107.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 C12 109.42(10) . . ?
C6 C10 C11 113.65(10) . . ?
C12 C10 C11 110.34(11) . . ?
C6 C10 H10A 107.7 . . ?
C12 C10 H10A 107.7 . . ?
C11 C10 H10A 107.7 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 N1 107.47(10) . . ?
N2 C13 C14 124.61(9) . . ?
N1 C13 C14 127.91(9) . . ?
C13 C14 C15 114.07(9) . . ?
C13 C14 C17 108.78(9) . . ?
C15 C14 C17 107.84(9) . . ?
C13 C14 C16 109.44(9) . . ?
C15 C14 C16 106.57(9) . . ?
C17 C14 C16 110.09(9) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Al1 C18 H18A 109.5 . . ?
Al1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Al1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Al1 C19 H19A 109.5 . . ?
Al1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Al1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C20 C20 107.60(11) . 3_766 ?
N2 C20 H20A 110.2 . . ?
C20 C20 H20A 110.2 3_766 . ?
N2 C20 H20B 110.2 . . ?
C20 C20 H20B 110.2 3_766 . ?
H20A C20 H20B 108.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al1 N2 1.9150(10) . ?
Al1 N1 1.9442(9) . ?
Al1 C19 1.9507(13) . ?
Al1 C18 1.9580(13) . ?
N2 C13 1.3379(14) . ?
N2 C20 1.4483(13) . ?
N1 C13 1.3478(14) . ?
N1 C1 1.4227(14) . ?
C1 C2 1.4084(16) . ?
C1 C6 1.4105(16) . ?
C2 C3 1.3926(16) . ?
C2 C7 1.5243(17) . ?
C3 C4 1.3811(19) . ?
C3 H3A 0.9500 . ?
C4 C5 1.3845(19) . ?
C4 H4A 0.9500 . ?
C5 C6 1.3915(16) . ?
C5 H5A 0.9500 . ?
C6 C10 1.5219(16) . ?
C7 C9 1.5344(18) . ?
C7 C8 1.5349(18) . ?
C7 H7A 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C12 1.5258(17) . ?
C10 C11 1.5325(17) . ?
C10 H10A 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.5345(15) . ?
C14 C15 1.5345(15) . ?
C14 C17 1.5389(15) . ?
C14 C16 1.5427(15) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C20 1.524(2) 3_766 ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
