#------------------------------------------------------------------------------
#$Date: 2025-08-20 21:19:29 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301836 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/33/4303310.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_4303310
loop_
_publ_author_name
'Suzanne C. Bart'
'Frank W. Heinemann'
'Christian Anthon'
'Christina Hauser'
'Karsten Meyer'
_publ_contact_author
;                                                                               
        Prof. Dr. K. Meyer       
        Department of Chemistry and Pharmacy
        Inorganic Chemistry
        Universität Erlangen-Nürnberg                   
        Egerlandstr. 1                                     
        D-91058 Erlangen                               
        Bundesrepublik Deutschland                             
;
_publ_contact_author_email       Karsten.Meyer@chemie.uni-erlangen.de
_publ_contact_author_fax         '049 9131 852-7367'
_publ_contact_author_phone       '049 9131 852-7360'
_publ_section_title
;
A New Tripodal Ligand System with Steric and Electronic Modularity for
Uranium Coordination Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9419
_journal_page_last               9426
_journal_paper_doi               10.1021/ic9012697
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C12 H15 Cl3'
_chemical_formula_sum            'C12 H15 Cl3'
_chemical_formula_weight         265.59
_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                117.915(6)
_cell_angle_beta                 108.127(3)
_cell_angle_gamma                102.038(6)
_cell_formula_units_Z            2
_cell_length_a                   9.2206(4)
_cell_length_b                   9.3069(8)
_cell_length_c                   9.3088(5)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     608.26(10)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
 ω-rotations with 2.00 ° and 12 sec per frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10411
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         3.50
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             276
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0368P)²+0.3492P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0851
_reflns_number_gt                2024
_reflns_number_total             2664
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9012697_si_001_2.cif
_cod_data_source_block           sd0735
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4303310
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
Cl1 Cl 0.47246(6) 0.37403(7) 0.61455(9) 0.03151(16) Uani 1 1 d . . .
Cl2 Cl -0.27909(7) -0.07117(7) -0.04659(7) 0.02965(15) Uani 1 1 d . . .
Cl3 Cl -0.19781(8) 0.25433(8) 0.81854(8) 0.03289(16) Uani 1 1 d . . .
C1 C 0.1621(2) 0.3642(3) 0.5735(3) 0.0178(4) Uani 1 1 d . . .
C2 C 0.0451(2) 0.3045(2) 0.3955(3) 0.0176(4) Uani 1 1 d . . .
C3 C -0.1239(2) 0.1957(2) 0.3236(3) 0.0165(4) Uani 1 1 d . . .
C4 C -0.1760(2) 0.1356(3) 0.4201(3) 0.0179(4) Uani 1 1 d . . .
C5 C -0.0560(2) 0.1868(3) 0.5917(3) 0.0173(4) Uani 1 1 d . . .
C6 C 0.1124(2) 0.3045(3) 0.6708(3) 0.0193(4) Uani 1 1 d . . .
C7 C 0.1012(3) 0.3572(3) 0.2843(3) 0.0246(5) Uani 1 1 d . . .
H7A H 0.0316 0.2605 0.1526 0.037 Uiso 1 1 calc R . .
H7B H 0.2194 0.3782 0.3204 0.037 Uiso 1 1 calc R . .
H7C H 0.0891 0.4671 0.3077 0.037 Uiso 1 1 calc R . .
C8 C -0.3600(3) 0.0215(3) 0.3411(3) 0.0252(5) Uani 1 1 d . . .
H8A H -0.4082 -0.0666 0.2079 0.038 Uiso 1 1 calc R . .
H8B H -0.4203 0.0982 0.3640 0.038 Uiso 1 1 calc R . .
H8C H -0.3707 -0.0410 0.4002 0.038 Uiso 1 1 calc R . .
C9 C 0.2394(3) 0.3669(3) 0.8613(3) 0.0301(5) Uani 1 1 d . . .
H9A H 0.3363 0.4768 0.9139 0.045 Uiso 1 1 calc R . .
H9B H 0.2772 0.2733 0.8512 0.045 Uiso 1 1 calc R . .
H9C H 0.1867 0.3910 0.9416 0.045 Uiso 1 1 calc R . .
C10 C 0.3405(2) 0.4921(3) 0.6564(3) 0.0231(5) Uani 1 1 d . . .
H10A H 0.3855 0.5774 0.7910 0.028 Uiso 1 1 calc R . .
H10B H 0.3431 0.5620 0.6025 0.028 Uiso 1 1 calc R . .
C11 C -0.2511(3) 0.1418(3) 0.1399(3) 0.0201(4) Uani 1 1 d . . .
H11A H -0.2134 0.2355 0.1200 0.024 Uiso 1 1 calc R . .
H11B H -0.3602 0.1321 0.1396 0.024 Uiso 1 1 calc R . .
C12 C -0.1091(3) 0.1183(3) 0.6932(3) 0.0228(5) Uani 1 1 d . . .
H12A H -0.0106 0.1227 0.7804 0.027 Uiso 1 1 calc R . .
H12B H -0.1937 -0.0079 0.6043 0.027 Uiso 1 1 calc R . .
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'
Cl Cl 0.1484 0.1585 '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
C6 C1 C2 120.49(18) . . ?
C6 C1 C10 120.61(18) . . ?
C2 C1 C10 118.91(18) . . ?
C3 C2 C1 118.88(18) . . ?
C3 C2 C7 120.52(18) . . ?
C1 C2 C7 120.60(18) . . ?
C2 C3 C4 121.13(18) . . ?
C2 C3 C11 119.22(18) . . ?
C4 C3 C11 119.65(17) . . ?
C5 C4 C3 119.11(18) . . ?
C5 C4 C8 120.91(18) . . ?
C3 C4 C8 119.96(18) . . ?
C4 C5 C6 120.48(18) . . ?
C4 C5 C12 119.61(18) . . ?
C6 C5 C12 119.89(18) . . ?
C1 C6 C5 119.66(18) . . ?
C1 C6 C9 120.30(18) . . ?
C5 C6 C9 120.04(19) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C1 C10 Cl1 111.29(14) . . ?
C1 C10 H10A 109.4 . . ?
Cl1 C10 H10A 109.4 . . ?
C1 C10 H10B 109.4 . . ?
Cl1 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C3 C11 Cl2 111.28(13) . . ?
C3 C11 H11A 109.4 . . ?
Cl2 C11 H11A 109.4 . . ?
C3 C11 H11B 109.4 . . ?
Cl2 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C5 C12 Cl3 109.83(14) . . ?
C5 C12 H12A 109.7 . . ?
Cl3 C12 H12A 109.7 . . ?
C5 C12 H12B 109.7 . . ?
Cl3 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
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
Cl1 C10 1.815(2) . ?
Cl2 C11 1.815(2) . ?
Cl3 C12 1.810(2) . ?
C1 C6 1.401(3) . ?
C1 C2 1.413(3) . ?
C1 C10 1.500(3) . ?
C2 C3 1.401(3) . ?
C2 C7 1.511(3) . ?
C3 C4 1.406(3) . ?
C3 C11 1.502(3) . ?
C4 C5 1.404(3) . ?
C4 C8 1.512(3) . ?
C5 C6 1.406(3) . ?
C5 C12 1.503(3) . ?
C6 C9 1.521(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
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 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 256883
2 PubChem 291188
