#------------------------------------------------------------------------------
#$Date: 2024-05-05 05:39:27 +0300 (Sun, 05 May 2024) $
#$Revision: 291610 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/56/7715685.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_7715685
loop_
_publ_author_name
'Borah, Aditya'
'Dey, Sourav'
'Siddiqui, Kehkasha'
'Gupta, Sandeep K.'
'Rajaraman, Gopalan'
'Murugavel, Ramaswamy'
_publ_section_title
;
 Magnetic anisotropy in octahedral Dy(III) and Yb(III) complexes.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7263
_journal_page_last               7267
_journal_paper_doi               10.1039/d3dt04352e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C72 H114 O24 P6 Yb, 3(H3 O2)'
_chemical_formula_sum            'C72 H123 O30 P6 Yb'
_chemical_formula_weight         1827.56
_chemical_name_systematic        2
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-11-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-21 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   23.5532(3)
_cell_length_b                   23.5532(3)
_cell_length_c                   13.4632(2)
_cell_measurement_reflns_used    6976
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.1090
_cell_measurement_theta_min      2.4910
_cell_volume                     6468.13(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn 724+ ccd diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14642
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.990
_diffrn_reflns_theta_max         24.990
_diffrn_reflns_theta_min         2.505
_exptl_absorpt_coefficient_mu    1.273
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             2865
_exptl_crystal_preparation       esi
_exptl_crystal_recrystallization_method esi
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0306
_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)+(0.0251P)²+14.8839P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2467
_reflns_number_total             2523
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt04352e3.cif
_cod_data_source_block           adi-yb-hexa
_cod_depositor_comments
'Adding full bibliography for 7715683--7715685.cif.'
_cod_original_cell_volume        6468.13(19)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7715685
_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_max   0.803
_shelx_estimated_absorpt_t_min   0.664
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Uiso: H3(0.08) H2(0.08) H5A(0.08) H5B(0.08)
 Fixed X: H5B(0.805901)
 Fixed Y: H5B(0.6906)
 Fixed Z: H5B(0.7818)
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_olex2_exptl_crystal_mounting_method esi
_olex2_submission_original_sample_id 2
_olex2_submission_special_instructions 'No special instructions were received'
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'
'-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
Yb1 Yb 0.666667 0.333333 0.833333 0.02493(11) Uani 1 6 d S T P . .
P1 P 0.68418(4) 0.48056(4) 0.72413(6) 0.03237(19) Uani 1 1 d . . . . .
H3 H 0.758(2) 0.565(2) 0.750(3) 0.080 Uiso 1 1 d . U . . .
O1 O 0.67145(10) 0.41335(9) 0.74254(15) 0.0366(5) Uani 1 1 d . . . . .
O2 O 0.62943(15) 0.49092(13) 0.7676(2) 0.0596(8) Uani 1 1 d . . . . .
H2 H 0.608(2) 0.470(2) 0.809(3) 0.080 Uiso 1 1 d . U . . .
O3 O 0.75042(14) 0.53317(11) 0.75901(18) 0.0518(7) Uani 1 1 d . . . . .
O4 O 0.67793(9) 0.48918(9) 0.60892(14) 0.0314(4) Uani 1 1 d . . . . .
O5 O 0.78917(16) 0.65266(14) 0.7259(3) 0.0903(10) Uani 1 1 d . . . . .
H5A H 0.833333 0.666667 0.666667 0.080 Uiso 1 2 d S U P . .
H5B H 0.805901 0.690600 0.781800 0.080 Uiso 1 1 d . U . . .
C1 C 0.72422(13) 0.53532(13) 0.5428(2) 0.0289(6) Uani 1 1 d . . . . .
C2 C 0.71566(14) 0.58774(14) 0.5164(2) 0.0327(7) Uani 1 1 d . . . . .
C3 C 0.75796(16) 0.63038(16) 0.4446(2) 0.0449(8) Uani 1 1 d . . . . .
H3A H 0.754170 0.667082 0.424959 0.054 Uiso 1 1 calc R U . . .
C4 C 0.80505(18) 0.62034(18) 0.4017(3) 0.0558(10) Uani 1 1 d . . . . .
H4 H 0.832938 0.649579 0.351948 0.067 Uiso 1 1 calc R U . . .
C5 C 0.81207(17) 0.56839(17) 0.4303(3) 0.0491(9) Uani 1 1 d . . . . .
H5 H 0.845210 0.562412 0.400222 0.059 Uiso 1 1 calc R U . . .
C6 C 0.77176(15) 0.52408(15) 0.5024(2) 0.0367(7) Uani 1 1 d . . . . .
C7 C 0.66157(16) 0.59671(15) 0.5619(2) 0.0390(7) Uani 1 1 d . . . . .
H7 H 0.654863 0.580176 0.631735 0.047 Uiso 1 1 calc R U . . .
C8 C 0.59779(18) 0.5551(2) 0.5056(3) 0.0619(10) Uani 1 1 d . . . . .
H8A H 0.603281 0.569692 0.436307 0.093 Uiso 1 1 calc R U . . .
H8B H 0.562702 0.559915 0.536363 0.093 Uiso 1 1 calc R U . . .
H8C H 0.586335 0.509014 0.507926 0.093 Uiso 1 1 calc R U . . .
C9 C 0.6776(2) 0.66778(18) 0.5652(3) 0.0662(11) Uani 1 1 d . . . . .
H9A H 0.719575 0.694405 0.599148 0.099 Uiso 1 1 calc R U . . .
H9B H 0.642949 0.670635 0.601294 0.099 Uiso 1 1 calc R U . . .
H9C H 0.680495 0.684066 0.497341 0.099 Uiso 1 1 calc R U . . .
C10 C 0.78224(16) 0.46817(16) 0.5342(2) 0.0412(7) Uani 1 1 d . . . . .
H10 H 0.745435 0.439522 0.579899 0.049 Uiso 1 1 calc R U . . .
C11 C 0.7798(2) 0.4259(2) 0.4469(3) 0.0736(12) Uani 1 1 d . . . . .
H11A H 0.738161 0.409598 0.411542 0.110 Uiso 1 1 calc R U . . .
H11B H 0.783544 0.388700 0.471430 0.110 Uiso 1 1 calc R U . . .
H11C H 0.816234 0.452150 0.401535 0.110 Uiso 1 1 calc R U . . .
C12 C 0.8457(2) 0.4933(2) 0.5925(3) 0.0677(11) Uani 1 1 d . . . . .
H12A H 0.882857 0.522448 0.550217 0.102 Uiso 1 1 calc R U . . .
H12B H 0.850492 0.456200 0.613885 0.102 Uiso 1 1 calc R U . . .
H12C H 0.844546 0.517592 0.650887 0.102 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 '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
O1 Yb1 O1 92.15(7) 3_665 2_655 ?
O1 Yb1 O1 92.15(7) 16_656 17_556 ?
O1 Yb1 O1 87.85(7) . 18_546 ?
O1 Yb1 O1 87.85(7) 3_665 16_656 ?
O1 Yb1 O1 180.0 3_665 18_546 ?
O1 Yb1 O1 87.85(7) 2_655 16_656 ?
O1 Yb1 O1 180.0 2_655 17_556 ?
O1 Yb1 O1 92.15(7) 3_665 . ?
O1 Yb1 O1 87.85(7) . 17_556 ?
O1 Yb1 O1 92.15(7) 2_655 . ?
O1 Yb1 O1 92.15(7) 16_656 18_546 ?
O1 Yb1 O1 180.0 16_656 . ?
O1 Yb1 O1 92.15(7) 17_556 18_546 ?
O1 Yb1 O1 87.85(7) 3_665 17_556 ?
O1 Yb1 O1 87.85(7) 2_655 18_546 ?
O1 P1 H3 132.7(14) . . ?
O1 P1 O2 111.60(13) . . ?
O1 P1 O3 113.70(13) . . ?
O1 P1 O4 108.67(11) . . ?
O2 P1 H3 99.3(14) . . ?
O2 P1 O4 102.30(13) . . ?
O3 P1 H3 19.0(14) . . ?
O3 P1 O2 110.89(17) . . ?
O3 P1 O4 109.01(12) . . ?
O4 P1 H3 98.1(14) . . ?
P1 O1 Yb1 155.03(13) . . ?
P1 O2 H2 122(3) . . ?
P1 O3 H3 115(4) . . ?
C1 O4 P1 129.36(17) . . ?
H5A O5 H5B 108.9(2) . . ?
C2 C1 O4 116.5(2) . . ?
C6 C1 O4 119.3(2) . . ?
C6 C1 C2 123.9(3) . . ?
C1 C2 C7 121.6(3) . . ?
C3 C2 C1 116.6(3) . . ?
C3 C2 C7 121.8(3) . . ?
C2 C3 H3A 119.4 . . ?
C4 C3 C2 121.1(3) . . ?
C4 C3 H3A 119.4 . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.3(3) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 119.2 . . ?
C4 C5 C6 121.6(3) . . ?
C6 C5 H5 119.2 . . ?
C1 C6 C5 116.4(3) . . ?
C1 C6 C10 123.5(3) . . ?
C5 C6 C10 120.1(3) . . ?
C2 C7 H7 107.7 . . ?
C2 C7 C8 109.7(3) . . ?
C2 C7 C9 113.6(3) . . ?
C8 C7 H7 107.7 . . ?
C9 C7 H7 107.7 . . ?
C9 C7 C8 110.1(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 H10 107.3 . . ?
C6 C10 C11 112.3(3) . . ?
C6 C10 C12 111.2(3) . . ?
C11 C10 H10 107.3 . . ?
C12 C10 H10 107.3 . . ?
C12 C10 C11 111.2(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
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
Yb1 O1 2.2015(18) 3_665 ?
Yb1 O1 2.2015(18) 17_556 ?
Yb1 O1 2.2014(18) . ?
Yb1 O1 2.2015(18) 2_655 ?
Yb1 O1 2.2016(18) 16_656 ?
Yb1 O1 2.2014(18) 18_546 ?
P1 H3 1.90(5) . ?
P1 O1 1.477(2) . ?
P1 O2 1.542(2) . ?
P1 O3 1.502(3) . ?
P1 O4 1.581(2) . ?
O2 H2 0.75(4) . ?
O3 H3 0.69(4) . ?
O4 C1 1.406(3) . ?
O5 H5A 1.218(4) . ?
O5 H5B 1.081(3) . ?
C1 C2 1.393(4) . ?
C1 C6 1.385(4) . ?
C2 C3 1.391(4) . ?
C2 C7 1.520(4) . ?
C3 H3A 0.9500 . ?
C3 C4 1.372(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.369(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.394(4) . ?
C6 C10 1.518(4) . ?
C7 H7 1.0000 . ?
C7 C8 1.523(5) . ?
C7 C9 1.522(5) . ?
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 H10 1.0000 . ?
C10 C11 1.524(5) . ?
C10 C12 1.521(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
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
_geom_torsion_publ_flag
P1 O4 C1 C2 -102.1(3) . . . . ?
P1 O4 C1 C6 82.7(3) . . . . ?
O1 P1 O4 C1 -122.6(2) . . . . ?
O2 P1 O1 Yb1 -75.6(3) . . . . ?
O2 P1 O4 C1 119.3(2) . . . . ?
O3 P1 O1 Yb1 50.8(3) . . . . ?
O3 P1 O4 C1 1.8(3) . . . . ?
O4 P1 O1 Yb1 172.4(3) . . . . ?
O4 C1 C2 C3 -174.6(3) . . . . ?
O4 C1 C2 C7 3.7(4) . . . . ?
O4 C1 C6 C5 174.0(3) . . . . ?
O4 C1 C6 C10 -7.4(4) . . . . ?
C1 C2 C3 C4 0.7(5) . . . . ?
C1 C2 C7 C8 -83.9(3) . . . . ?
C1 C2 C7 C9 152.4(3) . . . . ?
C1 C6 C10 C11 125.7(4) . . . . ?
C1 C6 C10 C12 -109.0(4) . . . . ?
C2 C1 C6 C5 -0.8(5) . . . . ?
C2 C1 C6 C10 177.8(3) . . . . ?
C2 C3 C4 C5 -1.1(6) . . . . ?
C3 C2 C7 C8 94.4(4) . . . . ?
C3 C2 C7 C9 -29.3(4) . . . . ?
C3 C4 C5 C6 0.6(6) . . . . ?
C4 C5 C6 C1 0.4(5) . . . . ?
C4 C5 C6 C10 -178.3(3) . . . . ?
C5 C6 C10 C11 -55.8(4) . . . . ?
C5 C6 C10 C12 69.5(4) . . . . ?
C6 C1 C2 C3 0.3(4) . . . . ?
C6 C1 C2 C7 178.6(3) . . . . ?
C7 C2 C3 C4 -177.6(3) . . . . ?
