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#$Date: 2022-03-29 11:28:36 +0300 (Tue, 29 Mar 2022) $
#$Revision: 274077 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/49/8104923.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_8104923
loop_
_publ_author_name
'Hickson, Matthew'
'Sephton, Abigail'
'Dugmore, Travis'
'Hosten, Eric C.'
'Betz, Richard'
_publ_section_title
;
 The crystal structure of aqua-tris (1,3-diphenylpropane-1,3-dionato-κ2
 O,O′)-lanthanum(III), C45H35LaO7
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              205
_journal_page_last               207
_journal_paper_doi               10.1515/ncrs-2020-0504
_journal_volume                  236
_journal_year                    2021
_chemical_formula_sum            'C45 H35 La O7'
_chemical_formula_weight         826.64
_chemical_name_common
;
aqua-tris(1,3-diphenylpropane-1,3-dionato)-lanthanum(iii)
;
_chemical_name_systematic
;
aqua-tris(1,3-diphenylpropane-1,3-dionato)-lanthanum(iii)
;
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     SHELXS
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   22.3832(11)
_cell_length_b                   22.3832(11)
_cell_length_c                   6.4522(3)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      3.15
_cell_volume                     2799.5(2)
_computing_cell_refinement       'SAINT [1]'
_computing_data_collection       'APEX2 [1]'
_computing_data_reduction        'SAINT [1]'
_computing_molecular_graphics    'ORTEP3 [3], Mercury [4]'
_computing_publication_material  'SHELXL-97 [2], PLATON [5]'
_computing_structure_refinement  'SHELXL-97 [2]'
_computing_structure_solution    'SHELXS-97 [2]'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            14463
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.311
_diffrn_reflns_theta_min         3.153
_exptl_absorpt_coefficient_mu    1.197
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7730
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;                                                              
SADABS [6]                                         
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       rod
_exptl_crystal_F_000             1254
_exptl_crystal_size_max          0.516
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;	
Flack, H. D. (1983)                                                        
Acta Cryst. A39, 882--892.    				   
;
_refine_ls_abs_structure_Flack   0.001(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3097
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0193
_refine_ls_R_factor_gt           0.0192
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0261P)²+0.5136P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0462
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                3093
_reflns_number_total             3097
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0504_suppl.cif
_cod_data_source_block           g
_cod_original_cell_volume        2799.5(3)
_cod_database_code               8104923
_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.
;
_iucr_geom_bonds_special_details
;                                                              
Cg(1) is the centroid of carbon atoms C(11)-C(16).               
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
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
La1 La 0.666667 0.333333 0.67076(2) 0.02874(7) Uani 1 3 d S T P . .
O1 O 0.61972(12) 0.40750(11) 0.7561(3) 0.0357(4) Uani 1 1 d . . . . .
O2 O 0.57855(12) 0.31842(13) 0.4182(3) 0.0390(5) Uani 1 1 d . . . . .
O3 O 0.666667 0.333333 1.0621(5) 0.0381(8) Uani 1 3 d DS T P . .
H3A H 0.640070 0.338242 1.143943 0.057 Uiso 0.3333 1 d DR U P . .
H3B H 0.691164 0.323583 1.137802 0.057 Uiso 0.3333 1 d DR U P . .
C1 C 0.57855(15) 0.42455(14) 0.6797(4) 0.0297(6) Uani 1 1 d . . . . .
C2 C 0.53751(17) 0.39387(16) 0.5044(5) 0.0362(6) Uani 1 1 d . . . . .
H2 H 0.506380 0.408978 0.464301 0.043 Uiso 1 1 calc R U . . .
C3 C 0.53902(14) 0.34292(14) 0.3849(4) 0.0276(5) Uani 1 1 d . . . . .
C11 C 0.57458(15) 0.48210(14) 0.7856(4) 0.0313(6) Uani 1 1 d . . . . .
C12 C 0.60185(16) 0.50134(17) 0.9837(5) 0.0370(6) Uani 1 1 d . . . . .
H12 H 0.619639 0.476030 1.052617 0.044 Uiso 1 1 calc R U . . .
C13 C 0.60331(17) 0.5572(2) 1.0820(6) 0.0484(9) Uani 1 1 d . . . . .
H13 H 0.621890 0.569906 1.217706 0.058 Uiso 1 1 calc R U . . .
C14 C 0.57781(18) 0.59443(19) 0.9827(7) 0.0527(10) Uani 1 1 d . . . . .
H14 H 0.580579 0.633768 1.048075 0.063 Uiso 1 1 calc R U . . .
C15 C 0.5485(2) 0.57482(18) 0.7905(6) 0.0482(8) Uani 1 1 d . . . . .
H15 H 0.529393 0.599442 0.724954 0.058 Uiso 1 1 calc R U . . .
C16 C 0.54685(18) 0.51887(17) 0.6911(5) 0.0405(7) Uani 1 1 d . . . . .
H16 H 0.526598 0.505555 0.557454 0.049 Uiso 1 1 calc R U . . .
C21 C 0.49276(14) 0.31523(14) 0.1992(4) 0.0290(5) Uani 1 1 d . . . . .
C22 C 0.4510(2) 0.3403(2) 0.1316(7) 0.0568(11) Uani 1 1 d . . . . .
H22 H 0.449582 0.375902 0.207513 0.068 Uiso 1 1 calc R U . . .
C23 C 0.4111(2) 0.3143(2) -0.0456(7) 0.0623(12) Uani 1 1 d . . . . .
H23 H 0.382853 0.332489 -0.089486 0.075 Uiso 1 1 calc R U . . .
C24 C 0.41179(19) 0.2634(2) -0.1568(6) 0.0501(9) Uani 1 1 d . . . . .
H24 H 0.382422 0.244102 -0.273596 0.060 Uiso 1 1 calc R U . . .
C25 C 0.4554(2) 0.2403(2) -0.0988(7) 0.0597(11) Uani 1 1 d . . . . .
H25 H 0.458673 0.206814 -0.181034 0.072 Uiso 1 1 calc R U . . .
C26 C 0.49482(19) 0.2653(2) 0.0797(6) 0.0485(9) Uani 1 1 d . . . . .
H26 H 0.523847 0.247681 0.120231 0.058 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 '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
O1 La1 O1 115.02(4) . 3_665
O1 La1 O1 115.02(4) . 2_655
O1 La1 O1 115.02(4) 3_665 2_655
O1 La1 O2 149.07(8) . 2_655
O1 La1 O2 86.81(8) 3_665 2_655
O1 La1 O2 69.53(7) 2_655 2_655
O1 La1 O2 69.53(7) . .
O1 La1 O2 149.07(8) 3_665 .
O1 La1 O2 86.81(8) 2_655 .
O2 La1 O2 80.55(8) 2_655 .
O1 La1 O2 86.81(8) . 3_665
O1 La1 O2 69.53(7) 3_665 3_665
O1 La1 O2 149.07(8) 2_655 3_665
O2 La1 O2 80.56(8) 2_655 3_665
O2 La1 O2 80.55(8) . 3_665
O1 La1 O3 76.90(5) . .
O1 La1 O3 76.90(5) 3_665 .
O1 La1 O3 76.90(5) 2_655 .
O2 La1 O3 131.71(6) 2_655 .
O2 La1 O3 131.71(6) . .
O2 La1 O3 131.71(6) 3_665 .
C1 O1 La1 138.49(18) . .
C3 O2 La1 137.77(18) . .
La1 O3 H3A 128.8 . .
La1 O3 H3B 125.5 . .
H3A O3 H3B 105.4 . .
La1 O3 H3A 128.770(2) . 2_655
H3A O3 H3A 84.9 . 2_655
La1 O3 H3A 128.770(3) . 3_665
H3A O3 H3A 84.9 . 3_665
H3B O3 H3A 52.8 . 3_665
H3A O3 H3A 84.9 2_655 3_665
La1 O3 H3B 125.511(3) . 2_655
H3A O3 H3B 52.8 . 2_655
H3B O3 H3B 89.7 . 2_655
H3A O3 H3B 105.4 2_655 2_655
La1 O3 H3B 125.513(2) . 3_665
H3B O3 H3B 89.7 . 3_665
H3A O3 H3B 52.8 2_655 3_665
H3A O3 H3B 105.4 3_665 3_665
H3B O3 H3B 89.6 2_655 3_665
O1 C1 C2 124.5(3) . .
O1 C1 C11 116.6(2) . .
C2 C1 C11 118.9(3) . .
C3 C2 C1 124.8(3) . .
C3 C2 H2 117.6 . .
C1 C2 H2 117.6 . .
O2 C3 C2 124.6(3) . .
O2 C3 C21 116.2(2) . .
C2 C3 C21 119.1(3) . .
C12 C11 C16 118.4(3) . .
C12 C11 C1 118.7(3) . .
C16 C11 C1 122.9(3) . .
C13 C12 C11 120.5(3) . .
C13 C12 H12 119.7 . .
C11 C12 H12 119.7 . .
C14 C13 C12 120.1(3) . .
C14 C13 H13 120.0 . .
C12 C13 H13 120.0 . .
C15 C14 C13 120.2(3) . .
C15 C14 H14 119.9 . .
C13 C14 H14 119.9 . .
C14 C15 C16 120.0(4) . .
C14 C15 H15 120.0 . .
C16 C15 H15 120.0 . .
C15 C16 C11 120.7(3) . .
C15 C16 H16 119.7 . .
C11 C16 H16 119.7 . .
C26 C21 C22 117.2(3) . .
C26 C21 C3 119.1(3) . .
C22 C21 C3 123.6(3) . .
C21 C22 C23 121.1(3) . .
C21 C22 H22 119.5 . .
C23 C22 H22 119.5 . .
C24 C23 C22 120.9(4) . .
C24 C23 H23 119.5 . .
C22 C23 H23 119.5 . .
C23 C24 C25 119.0(3) . .
C23 C24 H24 120.5 . .
C25 C24 H24 120.5 . .
C24 C25 C26 120.3(3) . .
C24 C25 H25 119.8 . .
C26 C25 H25 119.8 . .
C21 C26 C25 121.3(3) . .
C21 C26 H26 119.3 . .
C25 C26 H26 119.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La1 O1 2.431(2) .
La1 O1 2.431(2) 3_665
La1 O1 2.431(2) 2_655
La1 O2 2.449(2) 2_655
La1 O2 2.449(2) .
La1 O2 2.449(2) 3_665
La1 O3 2.525(3) .
O1 C1 1.261(4) .
O2 C3 1.271(4) .
O3 H3A 0.8429 .
O3 H3B 0.8404 .
O3 H3A 0.8429 2_655
O3 H3A 0.8429 3_665
O3 H3B 0.8405 2_655
O3 H3B 0.8405 3_665
C1 C2 1.401(4) .
C1 C11 1.500(4) .
C2 C3 1.391(4) .
C2 H2 0.9500 .
C3 C21 1.500(4) .
C11 C12 1.389(4) .
C11 C16 1.395(5) .
C12 C13 1.388(5) .
C12 H12 0.9500 .
C13 C14 1.380(6) .
C13 H13 0.9500 .
C14 C15 1.368(6) .
C14 H14 0.9500 .
C15 C16 1.391(5) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C21 C26 1.377(4) .
C21 C22 1.379(5) .
C22 C23 1.387(5) .
C22 H22 0.9500 .
C23 C24 1.353(6) .
C23 H23 0.9500 .
C24 C25 1.366(6) .
C24 H24 0.9500 .
C25 C26 1.387(5) .
C25 H25 0.9500 .
C26 H26 0.9500 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3A O2 0.84 2.15 2.936(2) 155.6 1_556
O3 H3B O2 0.84 2.24 2.936(2) 139.9 2_656
C14 H14 <i>C<i>~g~(1) 0.95 2.66 3.581(4) 162 6_565
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
La1 O1 C1 C2 7.9(5) . . . .
La1 O1 C1 C11 -171.61(19) . . . .
O1 C1 C2 C3 -3.4(5) . . . .
C11 C1 C2 C3 176.2(3) . . . .
La1 O2 C3 C2 1.4(5) . . . .
La1 O2 C3 C21 179.7(2) . . . .
C1 C2 C3 O2 -1.0(5) . . . .
C1 C2 C3 C21 -179.2(3) . . . .
O1 C1 C11 C12 -15.5(4) . . . .
C2 C1 C11 C12 164.9(3) . . . .
O1 C1 C11 C16 162.1(3) . . . .
C2 C1 C11 C16 -17.4(4) . . . .
C16 C11 C12 C13 -2.0(5) . . . .
C1 C11 C12 C13 175.8(3) . . . .
C11 C12 C13 C14 -0.2(5) . . . .
C12 C13 C14 C15 2.5(5) . . . .
C13 C14 C15 C16 -2.5(6) . . . .
C14 C15 C16 C11 0.2(5) . . . .
C12 C11 C16 C15 2.1(5) . . . .
C1 C11 C16 C15 -175.6(3) . . . .
O2 C3 C21 C26 0.9(4) . . . .
C2 C3 C21 C26 179.3(3) . . . .
O2 C3 C21 C22 -174.5(4) . . . .
C2 C3 C21 C22 3.9(5) . . . .
C26 C21 C22 C23 2.2(7) . . . .
C3 C21 C22 C23 177.7(4) . . . .
C21 C22 C23 C24 0.2(8) . . . .
C22 C23 C24 C25 -3.5(8) . . . .
C23 C24 C25 C26 4.3(8) . . . .
C22 C21 C26 C25 -1.4(6) . . . .
C3 C21 C26 C25 -177.1(4) . . . .
C24 C25 C26 C21 -1.9(7) . . . .
