#------------------------------------------------------------------------------
#$Date: 2020-12-06 10:44:58 +0200 (Sun, 06 Dec 2020) $
#$Revision: 259592 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/16/7241688.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_7241688
loop_
_publ_author_name
'Arumugam, Selvakumar'
'Reddy, Pulikanti Guruprasad'
'Francis, Maria'
'Kulkarni, Aditya'
'Roy, Sudipta'
'Mondal, Kartik Chandra'
_publ_section_title
;
 Highly fluorescent aryl-cyclopentadienyl ligands and their tetra-nuclear
 mixed metallic potassium--dysprosium clusters
;
_journal_issue                   65
_journal_name_full               'RSC Advances'
_journal_page_first              39366
_journal_page_last               39372
_journal_paper_doi               10.1039/D0RA05316C
_journal_volume                  10
_journal_year                    2020
_chemical_formula_sum            'C26 H24'
_chemical_formula_weight         336.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           45
_space_group_name_Hall           'I 2 -2c'
_space_group_name_H-M_alt        'I b a 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2020-05-29 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.059(2)
_cell_length_b                   22.2927(12)
_cell_length_c                   7.6696(3)
_cell_measurement_reflns_used    5713
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.60
_cell_volume                     3771.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14443
_diffrn_reflns_point_group_measured_fraction_full 0.912
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.245
_diffrn_reflns_theta_min         1.846
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             1440
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane'
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
 Flack x determined using 1130 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -2.1(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3393
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0386
_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)+(0.0558P)²+1.1470P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1011
_reflns_Friedel_coverage         0.659
_reflns_Friedel_fraction_full    0.810
_reflns_Friedel_fraction_max     0.772
_reflns_number_gt                2980
_reflns_number_total             3393
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ra05316c2.cif
_cod_data_source_block           shelx_CCDC1
_cod_original_cell_volume        3771.5(4)
_cod_database_code               7241688
_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   0.982
_shelx_estimated_absorpt_t_max   0.993
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1, -y+1, z+1/2'
'-x+1, y+1, 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
C1 C 0.09223(10) 0.19381(10) 0.1129(3) 0.0317(5) Uani 1 1 d . . . . .
C2 C 0.05462(10) 0.24117(10) 0.0772(3) 0.0307(5) Uani 1 1 d . . . . .
C3 C -0.00924(11) 0.22002(10) 0.0920(3) 0.0339(6) Uani 1 1 d . . . . .
H3A H -0.0310 0.2438 0.1775 0.041 Uiso 1 1 calc R U . . .
H3B H -0.0297 0.2237 -0.0193 0.041 Uiso 1 1 calc R U . . .
C4 C -0.00718(11) 0.15837(10) 0.1452(3) 0.0327(6) Uani 1 1 d . . . . .
C5 C 0.05441(11) 0.14135(11) 0.1597(3) 0.0348(6) Uani 1 1 d . . . . .
H5 H 0.0686 0.1038 0.1928 0.042 Uiso 1 1 calc R U . . .
C6 C 0.15880(10) 0.18896(10) 0.1037(3) 0.0293(5) Uani 1 1 d . . . . .
C7 C 0.18964(11) 0.14870(11) 0.2112(4) 0.0336(6) Uani 1 1 d . . . . .
H7 H 0.1678 0.1253 0.2897 0.040 Uiso 1 1 calc R U . . .
C8 C 0.25183(11) 0.14286(11) 0.2036(4) 0.0352(6) Uani 1 1 d . . . . .
H8 H 0.2710 0.1160 0.2781 0.042 Uiso 1 1 calc R U . . .
C9 C 0.28643(10) 0.17604(10) 0.0873(4) 0.0318(5) Uani 1 1 d . . . . .
C10 C 0.25598(11) 0.21555(11) -0.0220(4) 0.0359(6) Uani 1 1 d . . . . .
H10 H 0.2779 0.2383 -0.1017 0.043 Uiso 1 1 calc R U . . .
C11 C 0.19340(11) 0.22162(11) -0.0145(3) 0.0350(6) Uani 1 1 d . . . . .
H11 H 0.1742 0.2481 -0.0902 0.042 Uiso 1 1 calc R U . . .
C12 C 0.35408(11) 0.16921(13) 0.0803(4) 0.0433(7) Uani 1 1 d . . . . .
H12A H 0.3641 0.1323 0.0227 0.065 Uiso 1 1 calc R U . . .
H12B H 0.3701 0.1688 0.1967 0.065 Uiso 1 1 calc R U . . .
H12C H 0.3713 0.2022 0.0169 0.065 Uiso 1 1 calc R U . . .
C13 C 0.06783(11) 0.30448(10) 0.0393(3) 0.0297(5) Uani 1 1 d . . . . .
C14 C 0.11817(11) 0.33416(11) 0.1095(4) 0.0336(6) Uani 1 1 d . . . . .
H14 H 0.1453 0.3130 0.1789 0.040 Uiso 1 1 calc R U . . .
C15 C 0.12829(12) 0.39417(11) 0.0777(4) 0.0398(6) Uani 1 1 d . . . . .
H15 H 0.1623 0.4124 0.1260 0.048 Uiso 1 1 calc R U . . .
C16 C 0.08943(13) 0.42808(11) -0.0236(4) 0.0426(7) Uani 1 1 d . . . . .
C17 C 0.03939(13) 0.39913(12) -0.0940(4) 0.0441(7) Uani 1 1 d . . . . .
H17 H 0.0127 0.4205 -0.1642 0.053 Uiso 1 1 calc R U . . .
C18 C 0.02852(11) 0.33876(11) -0.0616(4) 0.0367(6) Uani 1 1 d . . . . .
H18 H -0.0059 0.3208 -0.1084 0.044 Uiso 1 1 calc R U . . .
C19 C 0.10112(16) 0.49397(14) -0.0568(6) 0.0682(10) Uani 1 1 d . . . . .
H19A H 0.0729 0.5176 0.0093 0.102 Uiso 1 1 calc R U . . .
H19B H 0.0961 0.5024 -0.1787 0.102 Uiso 1 1 calc R U . . .
H19C H 0.1417 0.5038 -0.0220 0.102 Uiso 1 1 calc R U . . .
C20 C -0.06020(11) 0.12131(11) 0.1843(3) 0.0325(5) Uani 1 1 d . . . . .
C21 C -0.11872(12) 0.14080(12) 0.1466(4) 0.0409(7) Uani 1 1 d . . . . .
H21 H -0.1240 0.1771 0.0886 0.049 Uiso 1 1 calc R U . . .
C22 C -0.16917(12) 0.10758(12) 0.1933(4) 0.0414(6) Uani 1 1 d . . . . .
H22 H -0.2076 0.1221 0.1666 0.050 Uiso 1 1 calc R U . . .
C23 C -0.16351(12) 0.05316(12) 0.2790(4) 0.0377(6) Uani 1 1 d . . . . .
C24 C -0.10559(12) 0.03287(12) 0.3142(4) 0.0457(7) Uani 1 1 d . . . . .
H24 H -0.1004 -0.0038 0.3703 0.055 Uiso 1 1 calc R U . . .
C25 C -0.05508(12) 0.06614(11) 0.2673(4) 0.0445(7) Uani 1 1 d . . . . .
H25 H -0.0167 0.0511 0.2920 0.053 Uiso 1 1 calc R U . . .
C26 C -0.21873(13) 0.01917(13) 0.3378(4) 0.0497(8) Uani 1 1 d . . . . .
H26A H -0.2451 0.0456 0.4012 0.075 Uiso 1 1 calc R U . . .
H26B H -0.2066 -0.0134 0.4119 0.075 Uiso 1 1 calc R U . . .
H26C H -0.2397 0.0036 0.2379 0.075 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'
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
C2 C1 C6 130.6(2) . . ?
C2 C1 C5 108.4(2) . . ?
C6 C1 C5 121.0(2) . . ?
C1 C2 C13 131.2(2) . . ?
C1 C2 C3 108.3(2) . . ?
C13 C2 C3 120.4(2) . . ?
C4 C3 C2 107.2(2) . . ?
C4 C3 H3A 110.3 . . ?
C2 C3 H3A 110.3 . . ?
C4 C3 H3B 110.3 . . ?
C2 C3 H3B 110.3 . . ?
H3A C3 H3B 108.5 . . ?
C5 C4 C3 108.0(2) . . ?
C5 C4 C20 126.9(2) . . ?
C3 C4 C20 125.0(2) . . ?
C4 C5 C1 108.1(2) . . ?
C4 C5 H5 126.0 . . ?
C1 C5 H5 126.0 . . ?
C11 C6 C7 117.0(2) . . ?
C11 C6 C1 122.6(2) . . ?
C7 C6 C1 120.3(2) . . ?
C8 C7 C6 121.4(2) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C7 C8 C9 121.6(2) . . ?
C7 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
C8 C9 C10 117.4(2) . . ?
C8 C9 C12 121.1(2) . . ?
C10 C9 C12 121.5(2) . . ?
C11 C10 C9 121.2(2) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C6 121.4(2) . . ?
C10 C11 H11 119.3 . . ?
C6 C11 H11 119.3 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C18 C13 C14 116.6(2) . . ?
C18 C13 C2 120.9(2) . . ?
C14 C13 C2 122.3(2) . . ?
C15 C14 C13 121.3(2) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C14 C15 C16 122.0(3) . . ?
C14 C15 H15 119.0 . . ?
C16 C15 H15 119.0 . . ?
C15 C16 C17 117.2(2) . . ?
C15 C16 C19 121.3(3) . . ?
C17 C16 C19 121.4(3) . . ?
C16 C17 C18 121.2(3) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C17 C18 C13 121.6(2) . . ?
C17 C18 H18 119.2 . . ?
C13 C18 H18 119.2 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C25 C20 C21 116.5(2) . . ?
C25 C20 C4 121.9(2) . . ?
C21 C20 C4 121.5(2) . . ?
C22 C21 C20 121.7(2) . . ?
C22 C21 H21 119.2 . . ?
C20 C21 H21 119.2 . . ?
C21 C22 C23 121.3(3) . . ?
C21 C22 H22 119.4 . . ?
C23 C22 H22 119.4 . . ?
C24 C23 C22 117.5(2) . . ?
C24 C23 C26 121.7(3) . . ?
C22 C23 C26 120.7(3) . . ?
C23 C24 C25 121.2(3) . . ?
C23 C24 H24 119.4 . . ?
C25 C24 H24 119.4 . . ?
C24 C25 C20 121.8(3) . . ?
C24 C25 H25 119.1 . . ?
C20 C25 H25 119.1 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 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
C1 C2 1.370(3) . ?
C1 C6 1.474(3) . ?
C1 C5 1.481(3) . ?
C2 C13 1.470(3) . ?
C2 C3 1.490(3) . ?
C3 C4 1.434(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.415(3) . ?
C4 C20 1.463(3) . ?
C5 H5 0.9300 . ?
C6 C11 1.391(4) . ?
C6 C7 1.396(3) . ?
C7 C8 1.379(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.387(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.390(4) . ?
C9 C12 1.501(3) . ?
C10 C11 1.388(3) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C18 1.391(3) . ?
C13 C14 1.400(3) . ?
C14 C15 1.378(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.382(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.388(4) . ?
C16 C19 1.513(4) . ?
C17 C18 1.389(4) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C25 1.389(4) . ?
C20 C21 1.392(4) . ?
C21 C22 1.384(4) . ?
C21 H21 0.9300 . ?
C22 C23 1.386(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.382(4) . ?
C23 C26 1.504(4) . ?
C24 C25 1.386(4) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
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
C6 C1 C2 C13 -8.6(4) . . . . ?
C5 C1 C2 C13 174.1(2) . . . . ?
C6 C1 C2 C3 174.8(2) . . . . ?
C5 C1 C2 C3 -2.5(3) . . . . ?
C1 C2 C3 C4 2.3(3) . . . . ?
C13 C2 C3 C4 -174.7(2) . . . . ?
C2 C3 C4 C5 -1.1(3) . . . . ?
C2 C3 C4 C20 176.5(2) . . . . ?
C3 C4 C5 C1 -0.4(3) . . . . ?
C20 C4 C5 C1 -177.9(2) . . . . ?
C2 C1 C5 C4 1.9(3) . . . . ?
C6 C1 C5 C4 -175.7(2) . . . . ?
C2 C1 C6 C11 -30.5(4) . . . . ?
C5 C1 C6 C11 146.6(2) . . . . ?
C2 C1 C6 C7 152.2(3) . . . . ?
C5 C1 C6 C7 -30.7(3) . . . . ?
C11 C6 C7 C8 1.7(4) . . . . ?
C1 C6 C7 C8 179.2(2) . . . . ?
C6 C7 C8 C9 -0.9(4) . . . . ?
C7 C8 C9 C10 -0.1(4) . . . . ?
C7 C8 C9 C12 -180.0(3) . . . . ?
C8 C9 C10 C11 0.2(4) . . . . ?
C12 C9 C10 C11 -180.0(2) . . . . ?
C9 C10 C11 C6 0.7(4) . . . . ?
C7 C6 C11 C10 -1.7(4) . . . . ?
C1 C6 C11 C10 -179.1(2) . . . . ?
C1 C2 C13 C18 152.7(3) . . . . ?
C3 C2 C13 C18 -31.1(4) . . . . ?
C1 C2 C13 C14 -30.9(4) . . . . ?
C3 C2 C13 C14 145.3(2) . . . . ?
C18 C13 C14 C15 -0.8(4) . . . . ?
C2 C13 C14 C15 -177.3(2) . . . . ?
C13 C14 C15 C16 0.3(4) . . . . ?
C14 C15 C16 C17 -0.3(4) . . . . ?
C14 C15 C16 C19 179.8(3) . . . . ?
C15 C16 C17 C18 0.9(4) . . . . ?
C19 C16 C17 C18 -179.3(3) . . . . ?
C16 C17 C18 C13 -1.5(4) . . . . ?
C14 C13 C18 C17 1.3(4) . . . . ?
C2 C13 C18 C17 177.9(2) . . . . ?
C5 C4 C20 C25 10.0(4) . . . . ?
C3 C4 C20 C25 -167.1(3) . . . . ?
C5 C4 C20 C21 -172.8(2) . . . . ?
C3 C4 C20 C21 10.1(4) . . . . ?
C25 C20 C21 C22 1.5(4) . . . . ?
C4 C20 C21 C22 -175.9(3) . . . . ?
C20 C21 C22 C23 -0.3(4) . . . . ?
C21 C22 C23 C24 -0.8(4) . . . . ?
C21 C22 C23 C26 176.6(3) . . . . ?
C22 C23 C24 C25 0.8(4) . . . . ?
C26 C23 C24 C25 -176.6(3) . . . . ?
C23 C24 C25 C20 0.5(5) . . . . ?
C21 C20 C25 C24 -1.6(4) . . . . ?
C4 C20 C25 C24 175.8(3) . . . . ?
