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#$Date: 2024-10-06 11:05:18 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295262 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/68/7716834.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_7716834
loop_
_publ_author_name
'Ito, Shunichiro'
'Tanaka, Kazuo'
'Chujo, Yoshiki'
_publ_section_title
;
 Effects of a central element on the photoluminescence properties of
 β-diketiminate complexes composed of group 13 elements.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14858
_journal_page_last               14865
_journal_paper_doi               10.1039/d4dt01689k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_sum            'C39 H45 Al Cl2 N2'
_chemical_formula_weight         639.65
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
;
2024-06-22 deposited with the CCDC.	2024-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.897(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.878(3)
_cell_length_b                   16.177(2)
_cell_length_c                   24.527(2)
_cell_measurement_reflns_used    595
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      57.56
_cell_measurement_theta_min      5.23
_cell_volume                     3520.6(13)
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2017)'
_computing_data_collection       'RAPID AUTO (Rigaku, 2017)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2017)'
_computing_molecular_graphics
'ShelXle (J. Appl. Cryst., 44, (2011) 1281-1284.)'
_computing_publication_material
'ShelXle (J. Appl. Cryst., 44, (2011) 1281-1284.)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Raxis Rapid'
_diffrn_measurement_method       'oscillation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1235
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            60564
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.085
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  1.4430
_exptl_absorpt_correction_T_min  0.7374
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane and hexane'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         8072
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1302
_refine_ls_R_factor_gt           0.1081
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0764P)²+16.7984P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2582
_refine_ls_wR_factor_ref         0.2748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6360
_reflns_number_total             8072
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01689k2.cif
_cod_data_source_block           LAlCl_a
_cod_depositor_comments
'Adding full bibliography for 7716834--7716836.cif.'
_cod_original_cell_volume        3520.6(14)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7716834
_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   0.911
_shelx_estimated_absorpt_t_max   0.911
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 0.74735(17) 0.30322(9) 0.75241(6) 0.0337(3) Uani 1 1 d . . . . .
Cl1 Cl 0.94289(15) 0.37914(10) 0.75664(6) 0.0499(4) Uani 1 1 d . . . . .
Cl2 Cl 0.80160(19) 0.17647(8) 0.75410(6) 0.0540(4) Uani 1 1 d . . . . .
N1 N 0.6295(4) 0.3339(2) 0.69115(16) 0.0304(8) Uani 1 1 d . . . . .
N2 N 0.6205(4) 0.3343(2) 0.80804(17) 0.0313(8) Uani 1 1 d . . . . .
C1 C 0.5554(5) 0.4064(3) 0.69615(19) 0.0299(9) Uani 1 1 d . . . . .
C2 C 0.5261(5) 0.4409(3) 0.74731(19) 0.0317(10) Uani 1 1 d . . . . .
H2 H 0.484533 0.495023 0.746294 0.038 Uiso 1 1 calc R U . . .
C3 C 0.5490(5) 0.4074(3) 0.7994(2) 0.0308(9) Uani 1 1 d . . . . .
C4 C 0.5016(5) 0.4556(3) 0.64768(19) 0.0320(10) Uani 1 1 d . . . . .
C5 C 0.4143(6) 0.4235(3) 0.6045(2) 0.0366(10) Uani 1 1 d . . . . .
H5 H 0.384784 0.367027 0.604977 0.044 Uiso 1 1 calc R U . . .
C6 C 0.3699(6) 0.4736(3) 0.5605(2) 0.0412(12) Uani 1 1 d . . . . .
H6 H 0.309439 0.451451 0.531370 0.049 Uiso 1 1 calc R U . . .
C7 C 0.4137(6) 0.5553(3) 0.5594(2) 0.0411(12) Uani 1 1 d . . . . .
H7 H 0.383622 0.589340 0.529409 0.049 Uiso 1 1 calc R U . . .
C8 C 0.5014(6) 0.5878(3) 0.6019(2) 0.0410(12) Uani 1 1 d . . . . .
H8 H 0.532947 0.643916 0.600842 0.049 Uiso 1 1 calc R U . . .
C9 C 0.5428(6) 0.5387(3) 0.6458(2) 0.0375(11) Uani 1 1 d . . . . .
H9 H 0.600505 0.561811 0.675361 0.045 Uiso 1 1 calc R U . . .
C10 C 0.4992(5) 0.4587(3) 0.8467(2) 0.0323(10) Uani 1 1 d . . . . .
C11 C 0.4111(5) 0.4292(3) 0.8892(2) 0.0351(10) Uani 1 1 d . . . . .
H11 H 0.375908 0.373763 0.888596 0.042 Uiso 1 1 calc R U . . .
C12 C 0.3753(6) 0.4812(3) 0.9321(2) 0.0395(11) Uani 1 1 d . . . . .
H12 H 0.315174 0.461190 0.960604 0.047 Uiso 1 1 calc R U . . .
C13 C 0.4274(6) 0.5627(3) 0.9335(2) 0.0397(11) Uani 1 1 d . . . . .
H13 H 0.403994 0.597771 0.963116 0.048 Uiso 1 1 calc R U . . .
C14 C 0.5128(6) 0.5921(3) 0.8918(2) 0.0395(11) Uani 1 1 d . . . . .
H14 H 0.546992 0.647717 0.892479 0.047 Uiso 1 1 calc R U . . .
C15 C 0.5491(6) 0.5409(3) 0.8488(2) 0.0365(11) Uani 1 1 d . . . . .
H15 H 0.608553 0.561777 0.820438 0.044 Uiso 1 1 calc R U . . .
C16 C 0.6465(5) 0.2954(3) 0.63810(19) 0.0317(10) Uani 1 1 d . . . . .
C17 C 0.7486(6) 0.3266(3) 0.6012(2) 0.0364(11) Uani 1 1 d . . . . .
C18 C 0.7600(7) 0.2859(3) 0.5507(2) 0.0425(12) Uani 1 1 d . . . . .
H18 H 0.828814 0.306133 0.525018 0.051 Uiso 1 1 calc R U . . .
C19 C 0.6743(7) 0.2181(3) 0.5379(2) 0.0485(14) Uani 1 1 d . . . . .
H19 H 0.682566 0.192288 0.503310 0.058 Uiso 1 1 calc R U . . .
C20 C 0.5765(7) 0.1872(3) 0.5749(2) 0.0451(13) Uani 1 1 d . . . . .
H20 H 0.516977 0.140365 0.565229 0.054 Uiso 1 1 calc R U . . .
C21 C 0.5618(6) 0.2228(3) 0.6265(2) 0.0388(11) Uani 1 1 d . . . . .
C22 C 0.6230(5) 0.2933(3) 0.8607(2) 0.0320(10) Uani 1 1 d . . . . .
C23 C 0.7225(6) 0.3187(3) 0.9029(2) 0.0352(10) Uani 1 1 d . . . . .
C24 C 0.7208(6) 0.2753(3) 0.9525(2) 0.0427(12) Uani 1 1 d . . . . .
H24 H 0.788475 0.290706 0.981498 0.051 Uiso 1 1 calc R U . . .
C25 C 0.6211(7) 0.2099(3) 0.9596(2) 0.0483(14) Uani 1 1 d . . . . .
H25 H 0.619865 0.181791 0.993627 0.058 Uiso 1 1 calc R U . . .
C26 C 0.5248(7) 0.1863(3) 0.9176(2) 0.0474(14) Uani 1 1 d . . . . .
H26 H 0.456197 0.142229 0.923126 0.057 Uiso 1 1 calc R U . . .
C27 C 0.5252(6) 0.2254(3) 0.8665(2) 0.0370(11) Uani 1 1 d . . . . .
C28 C 0.8523(6) 0.3995(3) 0.6130(2) 0.0373(11) Uani 1 1 d . . . . .
H28 H 0.821691 0.425519 0.647945 0.045 Uiso 1 1 calc R U . . .
C29 C 1.0161(6) 0.3702(4) 0.6205(2) 0.0475(13) Uani 1 1 d . . . . .
H29A H 1.022275 0.327394 0.648783 0.071 Uiso 1 1 calc R U . . .
H29B H 1.080127 0.417057 0.631537 0.071 Uiso 1 1 calc R U . . .
H29C H 1.050470 0.347487 0.586053 0.071 Uiso 1 1 calc R U . . .
C30 C 0.8379(7) 0.4647(3) 0.5678(2) 0.0453(12) Uani 1 1 d . . . . .
H30A H 0.879211 0.442654 0.534225 0.068 Uiso 1 1 calc R U . . .
H30B H 0.893823 0.514425 0.578991 0.068 Uiso 1 1 calc R U . . .
H30C H 0.731381 0.478657 0.561320 0.068 Uiso 1 1 calc R U . . .
C31 C 0.4575(6) 0.1855(3) 0.6674(2) 0.0418(12) Uani 1 1 d . . . . .
H31 H 0.503081 0.196301 0.704587 0.050 Uiso 1 1 calc R U . . .
C32 C 0.4422(8) 0.0906(3) 0.6611(3) 0.0557(16) Uani 1 1 d . . . . .
H32A H 0.376066 0.069176 0.688948 0.084 Uiso 1 1 calc R U . . .
H32B H 0.541895 0.064967 0.665429 0.084 Uiso 1 1 calc R U . . .
H32C H 0.399104 0.077739 0.624758 0.084 Uiso 1 1 calc R U . . .
C33 C 0.3029(7) 0.2246(4) 0.6654(3) 0.0556(15) Uani 1 1 d . . . . .
H33A H 0.311380 0.283061 0.675483 0.083 Uiso 1 1 calc R U . . .
H33B H 0.238130 0.196129 0.690959 0.083 Uiso 1 1 calc R U . . .
H33C H 0.258839 0.219975 0.628328 0.083 Uiso 1 1 calc R U . . .
C34 C 0.8341(6) 0.3894(3) 0.8974(2) 0.0378(11) Uani 1 1 d . . . . .
H34 H 0.810814 0.418344 0.862106 0.045 Uiso 1 1 calc R U . . .
C35 C 0.9932(6) 0.3554(4) 0.8957(2) 0.0510(14) Uani 1 1 d . . . . .
H35A H 1.019280 0.328038 0.930398 0.076 Uiso 1 1 calc R U . . .
H35B H 1.063864 0.400825 0.889794 0.076 Uiso 1 1 calc R U . . .
H35C H 0.999158 0.315426 0.865852 0.076 Uiso 1 1 calc R U . . .
C36 C 0.8213(7) 0.4525(3) 0.9437(2) 0.0475(13) Uani 1 1 d . . . . .
H36A H 0.717362 0.472772 0.944646 0.071 Uiso 1 1 calc R U . . .
H36B H 0.889389 0.498968 0.937448 0.071 Uiso 1 1 calc R U . . .
H36C H 0.848847 0.426085 0.978571 0.071 Uiso 1 1 calc R U . . .
C37 C 0.4188(6) 0.1950(3) 0.8207(2) 0.0423(12) Uani 1 1 d . . . . .
H37 H 0.461060 0.213365 0.785447 0.051 Uiso 1 1 calc R U . . .
C38 C 0.4064(8) 0.1004(3) 0.8190(3) 0.0569(16) Uani 1 1 d . . . . .
H38A H 0.362365 0.080552 0.852636 0.085 Uiso 1 1 calc R U . . .
H38B H 0.506981 0.076415 0.815475 0.085 Uiso 1 1 calc R U . . .
H38C H 0.342007 0.083929 0.787600 0.085 Uiso 1 1 calc R U . . .
C39 C 0.2650(7) 0.2334(4) 0.8247(3) 0.0531(15) Uani 1 1 d . . . . .
H39A H 0.196038 0.208458 0.797362 0.080 Uiso 1 1 calc R U . . .
H39B H 0.271969 0.292993 0.818119 0.080 Uiso 1 1 calc R U . . .
H39C H 0.227039 0.223700 0.861219 0.080 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'
Al Al 0.0645 0.0514 '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'
N N 0.0061 0.0033 '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 100.42(18) . . ?
N2 Al1 Cl2 113.03(14) . . ?
N1 Al1 Cl2 113.29(14) . . ?
N2 Al1 Cl1 108.66(14) . . ?
N1 Al1 Cl1 108.69(14) . . ?
Cl2 Al1 Cl1 112.06(9) . . ?
C1 N1 C16 121.2(4) . . ?
C1 N1 Al1 114.7(3) . . ?
C16 N1 Al1 122.3(3) . . ?
C3 N2 C22 122.0(4) . . ?
C3 N2 Al1 114.3(3) . . ?
C22 N2 Al1 122.4(3) . . ?
N1 C1 C2 122.1(4) . . ?
N1 C1 C4 122.2(4) . . ?
C2 C1 C4 115.7(4) . . ?
C3 C2 C1 129.5(4) . . ?
N2 C3 C2 122.3(4) . . ?
N2 C3 C10 120.6(4) . . ?
C2 C3 C10 117.0(4) . . ?
C5 C4 C9 118.4(4) . . ?
C5 C4 C1 124.1(4) . . ?
C9 C4 C1 117.5(4) . . ?
C4 C5 C6 120.4(5) . . ?
C7 C6 C5 120.0(5) . . ?
C6 C7 C8 120.1(5) . . ?
C9 C8 C7 119.8(5) . . ?
C8 C9 C4 121.2(5) . . ?
C15 C10 C11 118.5(4) . . ?
C15 C10 C3 116.8(4) . . ?
C11 C10 C3 124.6(4) . . ?
C12 C11 C10 120.1(4) . . ?
C11 C12 C13 120.3(5) . . ?
C14 C13 C12 119.8(5) . . ?
C13 C14 C15 120.4(5) . . ?
C14 C15 C10 120.9(5) . . ?
C17 C16 C21 121.4(4) . . ?
C17 C16 N1 120.9(4) . . ?
C21 C16 N1 117.6(4) . . ?
C16 C17 C18 117.9(5) . . ?
C16 C17 C28 124.1(4) . . ?
C18 C17 C28 118.0(5) . . ?
C19 C18 C17 121.5(5) . . ?
C18 C19 C20 120.0(5) . . ?
C19 C20 C21 122.0(5) . . ?
C20 C21 C16 117.1(5) . . ?
C20 C21 C31 120.9(5) . . ?
C16 C21 C31 122.0(4) . . ?
C23 C22 C27 122.0(4) . . ?
C23 C22 N2 121.0(4) . . ?
C27 C22 N2 117.0(4) . . ?
C22 C23 C24 117.9(5) . . ?
C22 C23 C34 123.5(4) . . ?
C24 C23 C34 118.6(5) . . ?
C25 C24 C23 120.9(5) . . ?
C26 C25 C24 119.9(5) . . ?
C25 C26 C27 121.7(5) . . ?
C26 C27 C22 117.5(5) . . ?
C26 C27 C37 119.4(5) . . ?
C22 C27 C37 123.0(4) . . ?
C17 C28 C30 111.1(4) . . ?
C17 C28 C29 110.5(4) . . ?
C30 C28 C29 110.8(4) . . ?
C33 C31 C21 112.7(5) . . ?
C33 C31 C32 109.6(5) . . ?
C21 C31 C32 112.4(5) . . ?
C35 C34 C23 109.8(4) . . ?
C35 C34 C36 110.7(5) . . ?
C23 C34 C36 111.7(4) . . ?
C39 C37 C27 111.1(5) . . ?
C39 C37 C38 110.4(5) . . ?
C27 C37 C38 112.6(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 1.867(4) . ?
Al1 N1 1.869(4) . ?
Al1 Cl2 2.1064(19) . ?
Al1 Cl1 2.126(2) . ?
N1 C1 1.352(6) . ?
N1 C16 1.455(6) . ?
N2 C3 1.355(6) . ?
N2 C22 1.452(6) . ?
C1 C2 1.406(7) . ?
C1 C4 1.497(6) . ?
C2 C3 1.398(7) . ?
C3 C10 1.505(6) . ?
C4 C5 1.392(7) . ?
C4 C9 1.393(6) . ?
C5 C6 1.396(7) . ?
C6 C7 1.378(7) . ?
C7 C8 1.385(8) . ?
C8 C9 1.379(7) . ?
C10 C15 1.401(6) . ?
C10 C11 1.406(7) . ?
C11 C12 1.392(7) . ?
C12 C13 1.397(7) . ?
C13 C14 1.378(7) . ?
C14 C15 1.387(7) . ?
C16 C17 1.396(7) . ?
C16 C21 1.419(7) . ?
C17 C18 1.409(7) . ?
C17 C28 1.517(7) . ?
C18 C19 1.366(8) . ?
C19 C20 1.371(9) . ?
C20 C21 1.401(7) . ?
C21 C31 1.513(8) . ?
C22 C23 1.399(7) . ?
C22 C27 1.410(7) . ?
C23 C24 1.404(7) . ?
C23 C34 1.522(7) . ?
C24 C25 1.393(8) . ?
C25 C26 1.373(9) . ?
C26 C27 1.403(7) . ?
C27 C37 1.526(7) . ?
C28 C30 1.533(7) . ?
C28 C29 1.534(7) . ?
C31 C33 1.511(8) . ?
C31 C32 1.548(7) . ?
C34 C35 1.518(7) . ?
C34 C36 1.533(7) . ?
C37 C39 1.506(8) . ?
C37 C38 1.534(7) . ?
