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#$Date: 2025-08-20 16:06:16 +0300 (Wed, 20 Aug 2025) $
#$Revision: 301830 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/07/51/4075144.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_4075144
loop_
_publ_author_name
'García, Felipe'
'Hopkins, Alexander D.'
'Kowenicki, Richard A.'
'McPartlin, Mary'
'Rogers, Michael C.'
'Silvia, Jared S.'
'Wright, Dominic S.'
_publ_section_title
;
 Syntheses and Structure of Heterometallic Complexes Containing Tripodal
 Group 13 Ligands [RE(2-py)3]-(E = Al, In)†
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2561
_journal_paper_doi               10.1021/om0600691
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C16 H15 Al Cl N3 Zn'
_chemical_formula_weight         377.11
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.73(3)
_cell_angle_beta                 70.83(3)
_cell_angle_gamma                65.04(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5575(17)
_cell_length_b                   9.2395(18)
_cell_length_c                   12.713(3)
_cell_measurement_reflns_used    9359
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.0
_cell_volume                     859.5(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7522
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.633
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+2.9358P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1301
_reflns_number_gt                2414
_reflns_number_total             2998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0600691si20060130_121303.cif
_cod_data_source_block           dw0521
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075144
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.61910(16) 0.94825(15) 0.68880(11) 0.0448(5) Uani 0.817(3) 1 d P A 1
Zn1 Zn 0.78572(10) 0.61835(9) 0.79168(6) 0.0430(3) Uani 0.817(3) 1 d P A 1
Cl1 Cl 0.9263(3) 0.3860(2) 0.85652(17) 0.0675(6) Uani 0.817(3) 1 d P A 1
C01 C 0.4889(6) 1.1632(6) 0.6237(5) 0.0839(16) Uani 0.817(3) 1 d P A 1
H01A H 0.3778 1.2280 0.6797 0.126 Uiso 0.817(3) 1 calc PR A 1
H01B H 0.4619 1.1425 0.5606 0.126 Uiso 0.817(3) 1 calc PR A 1
H01C H 0.5667 1.2184 0.6009 0.126 Uiso 0.817(3) 1 calc PR A 1
N1 N 0.7537(6) 0.8132(6) 0.8734(4) 0.0412(11) Uani 0.817(3) 1 d P A 1
N2 N 0.9389(5) 0.6503(5) 0.6377(4) 0.0376(10) Uani 0.817(3) 1 d P A 1
N3 N 0.5377(6) 0.6804(6) 0.7768(4) 0.0494(12) Uani 0.817(3) 1 d P A 1
C1 C 0.6812(6) 0.9559(6) 0.8277(4) 0.0428(12) Uani 0.817(3) 1 d P A 1
C2 C 0.8610(6) 0.7914(6) 0.5914(4) 0.0388(12) Uani 0.817(3) 1 d P A 1
C3 C 0.4689(6) 0.8222(6) 0.7300(4) 0.0321(10) Uani 0.817(3) 1 d P A 1
Zn1' Zn 0.61910(16) 0.94825(15) 0.68880(11) 0.0448(5) Uani 0.183(3) 1 d P A 2
Al1' Al 0.78572(10) 0.61835(9) 0.79168(6) 0.0430(3) Uani 0.183(3) 1 d P A 2
C01' C 0.9263(3) 0.3860(2) 0.85652(17) 0.0675(6) Uani 0.183(3) 1 d P A 2
H01D H 1.0419 0.3767 0.8574 0.101 Uiso 0.183(3) 1 calc PR A 2
H01E H 0.9448 0.3009 0.8094 0.101 Uiso 0.183(3) 1 calc PR A 2
H01F H 0.8534 0.3794 0.9309 0.101 Uiso 0.183(3) 1 calc PR A 2
Cl1' Cl 0.4889(6) 1.1632(6) 0.6237(5) 0.0839(16) Uani 0.183(3) 1 d P A 2
C1' C 0.7537(6) 0.8132(6) 0.8734(4) 0.0412(11) Uani 0.183(3) 1 d P A 2
C2' C 0.9389(5) 0.6503(5) 0.6377(4) 0.0376(10) Uani 0.183(3) 1 d P A 2
C3' C 0.5377(6) 0.6804(6) 0.7768(4) 0.0494(12) Uani 0.183(3) 1 d P A 2
N1' N 0.6812(6) 0.9559(6) 0.8277(4) 0.0428(12) Uani 0.183(3) 1 d P A 2
N2' N 0.8610(6) 0.7914(6) 0.5914(4) 0.0388(12) Uani 0.183(3) 1 d P A 2
N3' N 0.4689(6) 0.8222(6) 0.7300(4) 0.0321(10) Uani 0.183(3) 1 d P A 2
C12 C 0.6713(8) 1.0901(7) 0.8760(5) 0.0579(16) Uani 1 1 d . . .
H12 H 0.6225 1.1894 0.8473 0.069 Uiso 1 1 calc R A 1
C13 C 0.7333(9) 1.0785(9) 0.9671(5) 0.0646(19) Uani 1 1 d . A .
H13 H 0.7268 1.1691 0.9980 0.078 Uiso 1 1 calc R . .
C14 C 0.8028(8) 0.9341(9) 1.0096(5) 0.0614(17) Uani 1 1 d . . .
H14 H 0.8450 0.9237 1.0698 0.074 Uiso 1 1 calc R A .
C15 C 0.8094(7) 0.8058(8) 0.9627(4) 0.0508(15) Uani 1 1 d . A .
H15 H 0.8545 0.7072 0.9931 0.061 Uiso 1 1 calc R B 1
C22 C 0.9597(9) 0.8167(8) 0.4861(5) 0.0577(16) Uani 1 1 d . . .
H22 H 0.9094 0.9110 0.4523 0.069 Uiso 1 1 calc R A 1
C23 C 1.1321(10) 0.7033(11) 0.4307(5) 0.071(2) Uani 1 1 d . A .
H23 H 1.1966 0.7219 0.3601 0.086 Uiso 1 1 calc R . .
C24 C 1.2080(9) 0.5639(9) 0.4794(6) 0.0636(18) Uani 1 1 d . . .
H24 H 1.3241 0.4873 0.4434 0.076 Uiso 1 1 calc R A .
C25 C 1.1075(7) 0.5411(7) 0.5824(5) 0.0501(14) Uani 1 1 d . A .
H25 H 1.1571 0.4465 0.6161 0.060 Uiso 1 1 calc R C 1
C32 C 0.3028(7) 0.8722(8) 0.7154(5) 0.0539(15) Uani 1 1 d . . .
H32 H 0.2555 0.9704 0.6850 0.065 Uiso 1 1 calc R A 1
C33 C 0.2039(9) 0.7821(10) 0.7441(6) 0.0684(19) Uani 1 1 d . A .
H33 H 0.0925 0.8178 0.7317 0.082 Uiso 1 1 calc R . .
C34 C 0.2706(9) 0.6393(9) 0.7911(6) 0.0659(19) Uani 1 1 d . . .
H34 H 0.2048 0.5770 0.8123 0.079 Uiso 1 1 calc R A .
C35 C 0.4382(8) 0.5892(7) 0.8065(5) 0.0535(15) Uani 1 1 d . A .
H35 H 0.4852 0.4917 0.8378 0.064 Uiso 1 1 calc R 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'
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'
Zn Zn 0.2839 1.4301 '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
C2 Al1 C1 100.1(2)
C2 Al1 C3 103.1(2)
C1 Al1 C3 104.1(2)
C2 Al1 C01 118.2(2)
C1 Al1 C01 118.1(2)
C3 Al1 C01 111.22(19)
N3 Zn1 N1 103.28(19)
N3 Zn1 N2 104.21(18)
N1 Zn1 N2 97.93(17)
N3 Zn1 Cl1 120.94(16)
N1 Zn1 Cl1 115.12(14)
N2 Zn1 Cl1 112.38(14)
C15 N1 C1 120.7(5)
C15 N1 Zn1 123.9(4)
C1 N1 Zn1 115.3(3)
C25 N2 C2 120.5(5)
C25 N2 Zn1 123.4(4)
C2 N2 Zn1 116.0(3)
C35 N3 C3 118.7(5)
C35 N3 Zn1 125.5(4)
C3 N3 Zn1 115.8(3)
N1 C1 C12 116.8(5)
N1 C1 Al1 116.6(4)
C12 C1 Al1 126.3(5)
N2 C2 C22 117.8(5)
N2 C2 Al1 115.7(3)
C22 C2 Al1 126.4(4)
N3 C3 C32 119.6(5)
N3 C3 Al1 116.7(3)
C32 C3 Al1 123.7(4)
C1 C12 C13 121.3(6)
C14 C13 C12 119.4(6)
C13 C14 C15 118.5(6)
N1 C15 C14 123.3(6)
C2 C22 C23 120.8(6)
C24 C23 C22 120.3(6)
C25 C24 C23 117.8(6)
N2 C25 C24 122.8(6)
C33 C32 C3 122.1(6)
C32 C33 C34 119.3(6)
C35 C34 C33 118.5(6)
N3 C35 C34 121.8(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Al1 C2 2.009(5)
Al1 C1 2.019(5)
Al1 C3 1.999(5)
Al1 C01 2.075(5)
Zn1 N3 2.021(5)
Zn1 N1 2.034(4)
Zn1 N2 2.043(4)
Zn1 Cl1 2.210(2)
N1 C15 1.354(7)
N1 C1 1.366(7)
N2 C25 1.353(7)
N2 C2 1.369(6)
N3 C35 1.383(7)
N3 C3 1.361(7)
C1 C12 1.393(7)
C2 C22 1.388(7)
C3 C32 1.368(7)
C12 C13 1.402(9)
C13 C14 1.355(9)
C14 C15 1.347(8)
C22 C23 1.385(9)
C23 C24 1.370(10)
C24 C25 1.364(9)
C32 C33 1.370(9)
C33 C34 1.367(10)
C34 C35 1.385(9)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139105318
