#------------------------------------------------------------------------------
#$Date: 2019-12-17 10:04:41 +0200 (Tue, 17 Dec 2019) $
#$Revision: 245246 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/66/1556608.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_1556608
loop_
_publ_author_name
'Langley, S.K.'
'Vignesh, K.R.'
'Holton, K.'
'Benjamin, S.'
'Hix, G.B.'
'Phonsri, W.'
'Moubaraki, B.'
'Murray, K.S.'
'Rajaraman, G.'
_publ_section_title
;
 Mononuclear Dysprosium(III) Complexes with Triphenylphosphine Oxide
 Ligands: Controlling the Coordination Environment and Magnetic Anisotropy
;
_journal_name_full               Inorganics
_journal_page_first              61
_journal_paper_doi               10.3390/inorganics6020061
_journal_volume                  6
_journal_year                    2018
_chemical_formula_sum            'C72 H60 Dy N3 O13 P4'
_chemical_formula_weight         1461.61
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0038(8)
_cell_length_b                   16.5124(8)
_cell_length_c                   26.6249(10)
_cell_measurement_reflns_used    8964
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.11
_cell_volume                     7035.9(6)
_computing_cell_refinement       'Bruker Apex2 V2.0'
_computing_data_collection       'Bruker Apex2 V2.0'
_computing_data_reduction        'Bruker Apex2 V2.0'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'APEX X8'
_diffrn_measurement_method       'scans in phi and omega'
_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  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            68643
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    1.216
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2972
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.159
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         8081
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0637
_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)+(0.0746P)²+48.9081P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1853
_reflns_number_gt                6095
_reflns_number_total             8081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            2-__Dy_OPPh3_4_NO3_2__NO3_.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      Pccn
_cod_database_code               1556608
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z-1/2'
'x, -y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.7500 0.2500 0.207584(12) 0.02042(13) Uani 1 2 d S . .
P2 P 0.91192(10) 0.17066(9) 0.11771(5) 0.0251(3) Uani 1 1 d . . .
P1 P 0.59055(10) 0.22379(10) 0.30934(6) 0.0262(3) Uani 1 1 d . . .
O1 O 0.6713(3) 0.1332(2) 0.17624(15) 0.0270(9) Uani 1 1 d . . .
O2 O 0.7649(3) 0.1060(3) 0.23270(16) 0.0282(9) Uani 1 1 d . . .
O3 O 0.6948(3) 0.0076(3) 0.1977(2) 0.0427(12) Uani 1 1 d . . .
C1 C 0.5033(4) 0.1675(4) 0.2857(2) 0.0311(13) Uani 1 1 d . . .
O5 O 0.6519(2) 0.2424(3) 0.26783(15) 0.0278(9) Uani 1 1 d . . .
O6 O 0.8371(3) 0.1988(3) 0.14749(15) 0.0286(9) Uani 1 1 d . . .
N7 N 0.7095(3) 0.0798(3) 0.20213(19) 0.0282(11) Uani 1 1 d . . .
C26 C 0.9601(4) 0.0248(4) 0.0740(2) 0.0310(13) Uani 1 1 d . . .
H26 H 1.0159 0.0429 0.0784 0.037 Uiso 1 1 calc R . .
C19 C 1.0027(4) 0.1575(4) 0.1567(2) 0.0295(13) Uani 1 1 d . . .
C8 C 0.4727(4) 0.3269(5) 0.3523(2) 0.0389(16) Uani 1 1 d . . .
H8 H 0.4346 0.2829 0.3507 0.047 Uiso 1 1 calc R . .
C2 C 0.4863(4) 0.1696(4) 0.2346(2) 0.0341(14) Uani 1 1 d . . .
H2 H 0.5212 0.2000 0.2128 0.041 Uiso 1 1 calc R . .
C13 C 0.6353(4) 0.1629(4) 0.3588(2) 0.0296(13) Uani 1 1 d . . .
C20 C 0.9905(4) 0.1107(4) 0.2002(2) 0.0309(13) Uani 1 1 d . . .
H20 H 0.9367 0.0895 0.2074 0.037 Uiso 1 1 calc R . .
C7 C 0.5543(4) 0.3163(4) 0.3364(2) 0.0305(13) Uani 1 1 d . . .
C25 C 0.8932(4) 0.0731(4) 0.0897(2) 0.0280(13) Uani 1 1 d . . .
C27 C 0.9445(5) -0.0499(4) 0.0517(3) 0.0365(15) Uani 1 1 d . . .
H27 H 0.9897 -0.0827 0.0408 0.044 Uiso 1 1 calc R . .
C31 C 0.9331(4) 0.2413(4) 0.0676(2) 0.0318(14) Uani 1 1 d . . .
C21 C 1.0565(5) 0.0953(4) 0.2325(3) 0.0385(16) Uani 1 1 d . . .
H21 H 1.0479 0.0646 0.2622 0.046 Uiso 1 1 calc R . .
C6 C 0.4519(4) 0.1221(4) 0.3173(3) 0.0396(16) Uani 1 1 d . . .
H6 H 0.4636 0.1199 0.3522 0.048 Uiso 1 1 calc R . .
C5 C 0.3844(4) 0.0803(5) 0.2983(3) 0.0442(18) Uani 1 1 d . . .
H5 H 0.3497 0.0496 0.3201 0.053 Uiso 1 1 calc R . .
C24 C 1.0811(4) 0.1875(4) 0.1451(3) 0.0384(15) Uani 1 1 d . . .
H24 H 1.0897 0.2186 0.1155 0.046 Uiso 1 1 calc R . .
C36 C 0.9943(5) 0.2276(5) 0.0312(3) 0.0464(19) Uani 1 1 d . . .
H36 H 1.0281 0.1803 0.0329 0.056 Uiso 1 1 calc R . .
C28 C 0.8637(5) -0.0762(4) 0.0456(3) 0.0389(16) Uani 1 1 d . . .
H28 H 0.8534 -0.1273 0.0304 0.047 Uiso 1 1 calc R . .
C18 C 0.6540(4) 0.0814(4) 0.3488(3) 0.0361(15) Uani 1 1 d . . .
H18 H 0.6434 0.0594 0.3164 0.043 Uiso 1 1 calc R . .
C17 C 0.6877(5) 0.0332(5) 0.3859(3) 0.0417(16) Uani 1 1 d . . .
H17 H 0.6995 -0.0220 0.3789 0.050 Uiso 1 1 calc R . .
C30 C 0.8115(4) 0.0462(4) 0.0836(2) 0.0317(13) Uani 1 1 d . . .
H30 H 0.7662 0.0791 0.0944 0.038 Uiso 1 1 calc R . .
C3 C 0.4186(5) 0.1274(4) 0.2154(3) 0.0412(16) Uani 1 1 d . . .
H3 H 0.4071 0.1288 0.1804 0.049 Uiso 1 1 calc R . .
C14 C 0.6516(5) 0.1946(5) 0.4062(3) 0.0422(17) Uani 1 1 d . . .
H14 H 0.6392 0.2496 0.4135 0.051 Uiso 1 1 calc R . .
C16 C 0.7045(5) 0.0642(5) 0.4329(3) 0.0490(19) Uani 1 1 d . . .
H16 H 0.7284 0.0306 0.4581 0.059 Uiso 1 1 calc R . .
C29 C 0.7961(5) -0.0284(5) 0.0617(3) 0.0424(17) Uani 1 1 d . . .
H29 H 0.7404 -0.0471 0.0576 0.051 Uiso 1 1 calc R . .
C4 C 0.3676(4) 0.0832(4) 0.2474(3) 0.0444(18) Uani 1 1 d . . .
H4 H 0.3208 0.0547 0.2342 0.053 Uiso 1 1 calc R . .
C15 C 0.6864(6) 0.1443(5) 0.4431(3) 0.054(2) Uani 1 1 d . . .
H15 H 0.6977 0.1656 0.4756 0.065 Uiso 1 1 calc R . .
C12 C 0.6089(5) 0.3810(4) 0.3400(3) 0.0455(18) Uani 1 1 d . . .
H12 H 0.6649 0.3745 0.3288 0.055 Uiso 1 1 calc R . .
C32 C 0.8841(5) 0.3099(4) 0.0643(3) 0.0439(18) Uani 1 1 d . . .
H32 H 0.8416 0.3198 0.0885 0.053 Uiso 1 1 calc R . .
C22 C 1.1352(5) 0.1253(5) 0.2211(3) 0.0453(18) Uani 1 1 d . . .
H22 H 1.1808 0.1144 0.2429 0.054 Uiso 1 1 calc R . .
C9 C 0.4459(5) 0.4016(5) 0.3705(3) 0.049(2) Uani 1 1 d . . .
H9 H 0.3895 0.4085 0.3808 0.059 Uiso 1 1 calc R . .
C34 C 0.9576(6) 0.3509(5) -0.0098(3) 0.056(2) Uani 1 1 d . . .
H34 H 0.9660 0.3888 -0.0362 0.067 Uiso 1 1 calc R . .
C10 C 0.5009(6) 0.4655(5) 0.3736(3) 0.052(2) Uani 1 1 d . . .
H10 H 0.4824 0.5167 0.3854 0.062 Uiso 1 1 calc R . .
C11 C 0.5842(6) 0.4543(5) 0.3594(3) 0.054(2) Uani 1 1 d . . .
H11 H 0.6234 0.4971 0.3630 0.064 Uiso 1 1 calc R . .
C23 C 1.1477(5) 0.1711(5) 0.1779(3) 0.0481(19) Uani 1 1 d . . .
H23 H 1.2019 0.1915 0.1705 0.058 Uiso 1 1 calc R . .
C33 C 0.8975(6) 0.3645(5) 0.0254(3) 0.057(2) Uani 1 1 d . . .
H33 H 0.8642 0.4120 0.0233 0.069 Uiso 1 1 calc R . .
C35 C 1.0060(6) 0.2825(6) -0.0073(3) 0.061(2) Uani 1 1 d . . .
H35 H 1.0476 0.2728 -0.0320 0.073 Uiso 1 1 calc R . .
O4S O 0.2500 0.2500 0.3562(6) 0.146(15) Uani 0.50 2 d SPD . .
O1S O 0.6792(10) -0.1483(9) -0.0904(5) 0.030(4) Uani 0.25 1 d PDU A -1
O5S O 0.3117(5) 0.2797(9) 0.4189(6) 0.117(7) Uani 0.50 1 d PD . .
N2S N 0.2500 0.2500 0.4013(6) 0.146(16) Uani 0.50 2 d SPDU . .
N1S N 0.7151(12) -0.1689(10) -0.0530(6) 0.050(6) Uani 0.25 1 d PDU A -1
O2S O 0.709(3) -0.2402(12) -0.0448(12) 0.139(16) Uani 0.25 1 d PDU A -1
O3S O 0.6967(16) -0.1289(14) -0.0170(5) 0.065(6) Uani 0.25 1 d PDU A -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'
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'
Dy Dy -0.1892 4.4098 '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
O5 Dy1 O5 88.9(2) 2_655 .
O5 Dy1 O6 154.90(15) 2_655 2_655
O5 Dy1 O6 95.41(15) . 2_655
O5 Dy1 O6 95.41(15) 2_655 .
O5 Dy1 O6 154.90(15) . .
O6 Dy1 O6 91.1(2) 2_655 .
O5 Dy1 O1 80.81(15) 2_655 2_655
O5 Dy1 O1 130.22(14) . 2_655
O6 Dy1 O1 77.53(15) 2_655 2_655
O6 Dy1 O1 74.87(14) . 2_655
O5 Dy1 O1 130.22(14) 2_655 .
O5 Dy1 O1 80.81(15) . .
O6 Dy1 O1 74.87(14) 2_655 .
O6 Dy1 O1 77.53(15) . .
O1 Dy1 O1 140.18(19) 2_655 .
O5 Dy1 O2 79.73(15) 2_655 2_655
O5 Dy1 O2 78.09(14) . 2_655
O6 Dy1 O2 77.03(14) 2_655 2_655
O6 Dy1 O2 127.01(14) . 2_655
O1 Dy1 O2 52.18(13) 2_655 2_655
O1 Dy1 O2 142.81(13) . 2_655
O5 Dy1 O2 78.09(14) 2_655 .
O5 Dy1 O2 79.72(15) . .
O6 Dy1 O2 127.01(14) 2_655 .
O6 Dy1 O2 77.03(14) . .
O1 Dy1 O2 142.81(13) 2_655 .
O1 Dy1 O2 52.18(13) . .
O2 Dy1 O2 148.73(19) 2_655 .
O6 P2 C19 112.0(3) . .
O6 P2 C25 111.2(3) . .
C19 P2 C25 105.4(3) . .
O6 P2 C31 109.8(3) . .
C19 P2 C31 110.7(3) . .
C25 P2 C31 107.7(3) . .
O5 P1 C7 109.4(3) . .
O5 P1 C1 110.8(3) . .
C7 P1 C1 109.4(3) . .
O5 P1 C13 112.9(3) . .
C7 P1 C13 108.1(3) . .
C1 P1 C13 106.1(3) . .
N7 O1 Dy1 96.5(3) . .
N7 O2 Dy1 94.9(3) . .
C2 C1 C6 119.2(6) . .
C2 C1 P1 119.0(5) . .
C6 C1 P1 121.8(5) . .
P1 O5 Dy1 171.0(3) . .
P2 O6 Dy1 165.0(3) . .
O3 N7 O1 122.0(5) . .
O3 N7 O2 121.7(5) . .
O1 N7 O2 116.3(5) . .
C27 C26 C25 119.8(6) . .
C24 C19 C20 120.4(6) . .
C24 C19 P2 124.1(5) . .
C20 C19 P2 115.4(5) . .
C7 C8 C9 120.6(7) . .
C1 C2 C3 120.2(6) . .
C14 C13 C18 119.5(6) . .
C14 C13 P1 121.8(5) . .
C18 C13 P1 118.8(5) . .
C21 C20 C19 120.5(6) . .
C8 C7 C12 118.6(6) . .
C8 C7 P1 122.5(6) . .
C12 C7 P1 118.8(5) . .
C30 C25 C26 120.1(6) . .
C30 C25 P2 119.4(5) . .
C26 C25 P2 120.5(5) . .
C28 C27 C26 120.0(6) . .
C32 C31 C36 119.2(6) . .
C32 C31 P2 118.1(5) . .
C36 C31 P2 122.7(5) . .
C20 C21 C22 119.4(7) . .
C5 C6 C1 120.7(7) . .
C6 C5 C4 119.7(7) . .
C19 C24 C23 118.7(7) . .
C35 C36 C31 120.2(7) . .
C27 C28 C29 120.7(6) . .
C17 C18 C13 120.1(7) . .
C18 C17 C16 120.9(7) . .
C29 C30 C25 120.1(6) . .
C2 C3 C4 119.8(7) . .
C13 C14 C15 119.2(7) . .
C17 C16 C15 119.5(7) . .
C30 C29 C28 119.4(7) . .
C5 C4 C3 120.3(7) . .
C16 C15 C14 120.8(8) . .
C11 C12 C7 121.6(7) . .
C31 C32 C33 119.5(7) . .
C21 C22 C23 120.4(7) . .
C10 C9 C8 120.2(7) . .
C33 C34 C35 120.0(7) . .
C9 C10 C11 119.5(7) . .
C12 C11 C10 119.5(8) . .
C22 C23 C24 120.6(7) . .
C34 C33 C32 121.0(8) . .
C34 C35 C36 120.2(8) . .
O5S N2S O5S 133.8(3) 2 .
O5S N2S O4S 113.08(14) 2 .
O5S N2S O4S 113.08(14) . .
O3S N1S O2S 112(3) . .
O3S N1S O1S 112.93(14) . .
O2S N1S O1S 112.97(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O5 2.247(4) 2_655
Dy1 O5 2.247(4) .
Dy1 O6 2.284(4) 2_655
Dy1 O6 2.284(4) .
Dy1 O1 2.451(4) 2_655
Dy1 O1 2.451(4) .
Dy1 O2 2.481(4) 2_655
Dy1 O2 2.481(4) .
P2 O6 1.510(4) .
P2 C19 1.798(7) .
P2 C25 1.800(6) .
P2 C31 1.804(6) .
P1 O5 1.511(4) .
P1 C7 1.787(7) .
P1 C1 1.792(7) .
P1 C13 1.804(6) .
O1 N7 1.275(6) .
O2 N7 1.279(7) .
O3 N7 1.221(7) .
C1 C2 1.387(9) .
C1 C6 1.394(9) .
C26 C27 1.390(9) .
C26 C25 1.400(8) .
C19 C24 1.383(9) .
C19 C20 1.405(9) .
C8 C7 1.383(9) .
C8 C9 1.393(11) .
C2 C3 1.387(9) .
C13 C14 1.393(9) .
C13 C18 1.404(10) .
C20 C21 1.386(9) .
C7 C12 1.383(10) .
C25 C30 1.390(9) .
C27 C28 1.375(11) .
C31 C32 1.380(9) .
C31 C36 1.397(9) .
C21 C22 1.386(11) .
C6 C5 1.378(10) .
C5 C4 1.384(11) .
C24 C23 1.406(10) .
C36 C35 1.380(11) .
C28 C29 1.406(10) .
C18 C17 1.377(9) .
C17 C16 1.380(11) .
C30 C29 1.386(9) .
C3 C4 1.387(10) .
C14 C15 1.402(10) .
C16 C15 1.382(12) .
C12 C11 1.374(11) .
C32 C33 1.390(10) .
C22 C23 1.391(12) .
C9 C10 1.376(13) .
C34 C33 1.363(12) .
C34 C35 1.371(12) .
C10 C11 1.398(12) .
O4S N2S 1.1996(10) .
O1S N1S 1.1998(10) .
O5S N2S 1.1987(10) .
N2S O5S 1.1987(10) 2
N1S O3S 1.1997(10) .
N1S O2S 1.1997(10) .
