#------------------------------------------------------------------------------
#$Date: 2016-06-14 11:04:59 +0300 (Tue, 14 Jun 2016) $
#$Revision: 183455 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/55/7225522.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_7225522
loop_
_publ_author_name
'Jiang, Y.'
'Holmberg, R. J.'
'Habib, F.'
'Ungur, L.'
'Korobkov, I.'
'Chibotaru, L. F.'
'Murugesu, M.'
_publ_section_title
;
 Probing the structural and magnetic properties of a new family of
 centrosymmetric dinuclear lanthanide complexes
;
_journal_issue                   61
_journal_name_full               'RSC Adv.'
_journal_page_first              56668
_journal_paper_doi               10.1039/C6RA12070A
_journal_volume                  6
_journal_year                    2016
_chemical_formula_sum            'C38 H60 Ho2 N6 O14'
_chemical_formula_weight         1154.78
_chemical_name_systematic        3
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-09-22 deposited with the CCDC.
2016-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.908(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2891(8)
_cell_length_b                   8.3607(6)
_cell_length_c                   20.7052(15)
_cell_measurement_reflns_used    7947
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.64
_cell_volume                     2242.3(3)
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_collection       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_molecular_graphics    'SHELXTL, Bruker (2004)'
_computing_publication_material  'SHELXTL, Bruker (2004)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-03 (Sheldrick, 2003)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.974
_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  0.1324
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29357
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.389
_diffrn_reflns_theta_min         1.572
_exptl_absorpt_coefficient_mu    3.572
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         3.222
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5476
_refine_ls_number_restraints     408
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0528
_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)+(0.0478P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1116
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3951
_reflns_number_total             5476
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ra12070a2.cif
_cod_data_source_block           mm424
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               7225522
_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   0.695
_shelx_estimated_absorpt_t_max   0.965
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ho1 Ho 0.36536(2) 0.97187(3) 0.52461(2) 0.01608(9) Uani 1 1 d . U
O1 O 0.2957(3) 0.9775(5) 0.6154(2) 0.0217(9) Uani 1 1 d . U
O2 O 0.1457(4) 1.0823(6) 0.6667(2) 0.0321(11) Uani 1 1 d . U
O3 O 0.5326(3) 0.8747(5) 0.5352(2) 0.0188(9) Uani 1 1 d . U
O4 O 0.3515(3) 0.8259(5) 0.4253(2) 0.0239(10) Uani 1 1 d . U
O5 O 0.1984(3) 0.8861(6) 0.4899(2) 0.0287(10) Uani 1 1 d . U
O6 O 0.4559(3) 1.1650(5) 0.5957(2) 0.0249(10) Uani 1 1 d . U
H6A H 0.4775 1.1772 0.6427 0.037 Uiso 1 1 d R U
H6B H 0.5044 1.2232 0.5730 0.037 Uiso 1 1 d R U
O7 O 0.3522(4) 1.2537(5) 0.6845(2) 0.0331(12) Uani 1 1 d . U
H7D H 0.3112 1.1785 0.6704 0.040 Uiso 1 1 calc R U
N1 N 0.4002(4) 0.7145(6) 0.5805(3) 0.0208(11) Uani 1 1 d . U
N2 N 0.4898(4) 0.6294(6) 0.5734(3) 0.0222(11) Uani 1 1 d . U
N3 N 0.7238(4) 0.7743(6) 0.5320(3) 0.0238(11) Uani 1 1 d . U
C1 C 0.2366(4) 0.8687(7) 0.6339(3) 0.0194(12) Uani 1 1 d . U
C2 C 0.1523(5) 0.9207(8) 0.6611(3) 0.0258(14) Uani 1 1 d . U
C3 C 0.0860(5) 0.8125(9) 0.6793(4) 0.0339(17) Uani 1 1 d . U
H3A H 0.0282 0.8498 0.6950 0.041 Uiso 1 1 calc R U
C4 C 0.1026(6) 0.6481(9) 0.6750(4) 0.0415(19) Uani 1 1 d . U
H4A H 0.0563 0.5743 0.6879 0.050 Uiso 1 1 calc R U
C5 C 0.1850(5) 0.5937(9) 0.6524(4) 0.0333(17) Uani 1 1 d . U
H5A H 0.1976 0.4820 0.6510 0.040 Uiso 1 1 calc R U
C6 C 0.2521(5) 0.7037(7) 0.6307(3) 0.0208(13) Uani 1 1 d . U
C7 C 0.0767(6) 1.1430(10) 0.7050(4) 0.043(2) Uani 1 1 d . U
H7A H 0.0783 1.2601 0.7048 0.064 Uiso 1 1 calc R U
H7B H 0.0982 1.1041 0.7507 0.064 Uiso 1 1 calc R U
H7C H 0.0064 1.1060 0.6858 0.064 Uiso 1 1 calc R U
C8 C 0.3442(5) 0.6366(8) 0.6129(3) 0.0224(13) Uani 1 1 d . U
H8A H 0.3635 0.5300 0.6261 0.027 Uiso 1 1 calc R U
C9 C 0.5493(4) 0.7229(7) 0.5490(3) 0.0185(12) Uani 1 1 d . U
C10 C 0.6438(5) 0.6508(7) 0.5309(3) 0.0231(13) Uani 1 1 d . U
H10A H 0.6719 0.5649 0.5628 0.028 Uiso 1 1 calc R U
H10B H 0.6243 0.6026 0.4862 0.028 Uiso 1 1 calc R U
C11 C 0.7753(5) 0.8103(9) 0.6012(4) 0.0367(16) Uani 1 1 d . U
H11A H 0.7241 0.8494 0.6249 0.055 Uiso 1 1 calc R U
H11B H 0.8281 0.8925 0.6019 0.055 Uiso 1 1 calc R U
H11C H 0.8077 0.7130 0.6226 0.055 Uiso 1 1 calc R U
C12 C 0.8002(5) 0.7152(9) 0.4960(4) 0.0371(18) Uani 1 1 d . U
H12A H 0.7657 0.6917 0.4500 0.056 Uiso 1 1 calc R U
H12B H 0.8325 0.6176 0.5173 0.056 Uiso 1 1 calc R U
H12C H 0.8532 0.7970 0.4967 0.056 Uiso 1 1 calc R U
C13 C 0.2835(5) 0.7411(7) 0.3880(3) 0.0241(13) Uani 1 1 d . U
C14 C 0.1859(5) 0.7129(8) 0.3991(3) 0.0273(14) Uani 1 1 d . U
H14A H 0.1417 0.6413 0.3702 0.033 Uiso 1 1 calc R U
C15 C 0.1490(5) 0.7840(8) 0.4504(4) 0.0278(14) Uani 1 1 d . U
C16 C 0.3141(6) 0.6622(9) 0.3295(3) 0.0340(16) Uani 1 1 d . U
H16A H 0.3847 0.6935 0.3283 0.051 Uiso 1 1 calc R U
H16B H 0.2667 0.6962 0.2884 0.051 Uiso 1 1 calc R U
H16C H 0.3106 0.5457 0.3338 0.051 Uiso 1 1 calc R U
C17 C 0.0448(6) 0.7381(10) 0.4615(4) 0.043(2) Uani 1 1 d . U
H17A H 0.0305 0.7996 0.4987 0.064 Uiso 1 1 calc R U
H17B H 0.0441 0.6236 0.4714 0.064 Uiso 1 1 calc R U
H17C H -0.0082 0.7614 0.4214 0.064 Uiso 1 1 calc R U
C18 C 0.3680(7) 1.2630(10) 0.7534(4) 0.047(2) Uani 1 1 d . U
H18A H 0.4001 1.1628 0.7736 0.056 Uiso 1 1 calc R U
H18B H 0.3007 1.2757 0.7659 0.056 Uiso 1 1 calc R U
C19 C 0.4353(7) 1.3997(11) 0.7788(4) 0.056(2) Uani 1 1 d . U
H19A H 0.4469 1.4033 0.8273 0.083 Uiso 1 1 calc R U
H19B H 0.4022 1.4992 0.7601 0.083 Uiso 1 1 calc R U
H19C H 0.5016 1.3874 0.7661 0.083 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'
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'
Ho Ho -0.2175 4.6783 '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 Ho1 O5 73.79(15) . .
O1 Ho1 O3 119.04(15) . .
O5 Ho1 O3 139.24(16) . .
O1 Ho1 O6 73.22(14) . .
O5 Ho1 O6 137.95(15) . .
O3 Ho1 O6 80.53(14) . .
O1 Ho1 O4 139.75(14) . .
O5 Ho1 O4 71.55(14) . .
O3 Ho1 O4 77.82(14) . .
O6 Ho1 O4 146.78(13) . .
O1 Ho1 O3 142.76(14) . 3_676
O5 Ho1 O3 128.67(16) . 3_676
O3 Ho1 O3 66.31(17) . 3_676
O6 Ho1 O3 71.59(14) . 3_676
O4 Ho1 O3 76.73(14) . 3_676
O1 Ho1 N1 72.26(15) . .
O5 Ho1 N1 86.60(17) . .
O3 Ho1 N1 64.62(14) . .
O6 Ho1 N1 107.17(17) . .
O4 Ho1 N1 85.81(16) . .
O3 Ho1 N1 130.29(14) 3_676 .
O1 Ho1 N3 97.33(15) . 3_676
O5 Ho1 N3 78.48(16) . 3_676
O3 Ho1 N3 131.39(14) . 3_676
O6 Ho1 N3 80.61(17) . 3_676
O4 Ho1 N3 95.22(17) . 3_676
O3 Ho1 N3 65.28(14) 3_676 3_676
N1 Ho1 N3 163.84(15) . 3_676
O1 Ho1 Ho1 140.19(11) . 3_676
O5 Ho1 Ho1 145.52(11) . 3_676
O3 Ho1 Ho1 33.73(9) . 3_676
O6 Ho1 Ho1 73.25(9) . 3_676
O4 Ho1 Ho1 74.74(9) . 3_676
O3 Ho1 Ho1 32.59(10) 3_676 3_676
N1 Ho1 Ho1 98.05(11) . 3_676
N3 Ho1 Ho1 97.77(10) 3_676 3_676
C1 O1 Ho1 127.4(4) . .
C2 O2 C7 117.3(5) . .
C9 O3 Ho1 118.1(3) . .
C9 O3 Ho1 122.8(3) . 3_676
Ho1 O3 Ho1 113.69(17) . 3_676
C13 O4 Ho1 136.6(4) . .
C15 O5 Ho1 138.0(4) . .
C8 N1 N2 113.3(5) . .
C8 N1 Ho1 128.6(4) . .
N2 N1 Ho1 117.9(3) . .
C9 N2 N1 109.7(5) . .
C12 N3 C11 109.8(5) . .
C12 N3 C10 109.4(5) . .
C11 N3 C10 109.4(5) . .
C12 N3 Ho1 110.2(4) . 3_676
C11 N3 Ho1 109.9(4) . 3_676
C10 N3 Ho1 108.2(4) . 3_676
O1 C1 C6 124.4(5) . .
O1 C1 C2 118.5(5) . .
C6 C1 C2 117.1(5) . .
O2 C2 C3 125.0(5) . .
O2 C2 C1 114.0(5) . .
C3 C2 C1 121.0(6) . .
C2 C3 C4 120.7(6) . .
C5 C4 C3 120.0(6) . .
C4 C5 C6 120.1(7) . .
C1 C6 C5 120.9(5) . .
C1 C6 C8 122.0(5) . .
C5 C6 C8 116.7(6) . .
N1 C8 C6 123.4(6) . .
N2 C9 O3 125.6(5) . .
N2 C9 C10 118.0(5) . .
O3 C9 C10 116.3(5) . .
N3 C10 C9 110.6(5) . .
O4 C13 C14 124.1(6) . .
O4 C13 C16 116.7(5) . .
C14 C13 C16 119.1(6) . .
C13 C14 C15 123.6(6) . .
O5 C15 C14 124.1(6) . .
O5 C15 C17 116.0(6) . .
C14 C15 C17 119.9(7) . .
O7 C18 C19 110.4(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ho1 O1 2.274(4) .
Ho1 O5 2.290(4) .
Ho1 O3 2.330(4) .
Ho1 O6 2.331(4) .
Ho1 O4 2.363(4) .
Ho1 O3 2.402(4) 3_676
Ho1 N1 2.438(5) .
Ho1 N3 2.580(5) 3_676
Ho1 Ho1 3.9618(5) 3_676
O1 C1 1.313(7) .
O2 C2 1.360(9) .
O2 C7 1.434(7) .
O3 C9 1.308(7) .
O3 Ho1 2.402(4) 3_676
O4 C13 1.266(8) .
O5 C15 1.261(8) .
O7 C18 1.397(9) .
N1 C8 1.286(7) .
N1 N2 1.422(6) .
N2 C9 1.294(7) .
N3 C12 1.472(7) .
N3 C11 1.474(9) .
N3 C10 1.479(7) .
N3 Ho1 2.580(5) 3_676
C1 C6 1.398(8) .
C1 C2 1.430(8) .
C2 C3 1.373(9) .
C3 C4 1.398(10) .
C4 C5 1.362(9) .
C5 C6 1.422(8) .
C6 C8 1.466(8) .
C9 C10 1.513(8) .
C13 C14 1.387(8) .
C13 C16 1.514(9) .
C14 C15 1.399(9) .
C15 C17 1.503(9) .
C18 C19 1.474(11) .
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
C8 N1 N2 C9 -170.9(6) .
Ho1 N1 N2 C9 13.6(6) .
Ho1 O1 C1 C6 41.0(8) .
Ho1 O1 C1 C2 -140.9(5) .
C7 O2 C2 C3 11.9(10) .
C7 O2 C2 C1 -168.1(6) .
O1 C1 C2 O2 -2.1(9) .
C6 C1 C2 O2 176.0(6) .
O1 C1 C2 C3 177.9(6) .
C6 C1 C2 C3 -4.0(10) .
O2 C2 C3 C4 -176.5(7) .
C1 C2 C3 C4 3.5(11) .
C2 C3 C4 C5 -0.2(12) .
C3 C4 C5 C6 -2.3(12) .
O1 C1 C6 C5 179.4(6) .
C2 C1 C6 C5 1.4(10) .
O1 C1 C6 C8 7.1(10) .
C2 C1 C6 C8 -171.0(6) .
C4 C5 C6 C1 1.7(11) .
C4 C5 C6 C8 174.5(7) .
N2 N1 C8 C6 175.5(6) .
Ho1 N1 C8 C6 -9.6(10) .
C1 C6 C8 N1 -21.7(10) .
C5 C6 C8 N1 165.6(7) .
N1 N2 C9 O3 2.6(9) .
N1 N2 C9 C10 -173.9(5) .
Ho1 O3 C9 N2 -18.4(8) .
Ho1 O3 C9 N2 -170.8(5) 3_676
Ho1 O3 C9 C10 158.1(4) .
Ho1 O3 C9 C10 5.7(7) 3_676
C12 N3 C10 C9 -163.3(6) .
C11 N3 C10 C9 76.4(6) .
Ho1 N3 C10 C9 -43.2(6) 3_676
N2 C9 C10 N3 -155.5(6) .
O3 C9 C10 N3 27.7(8) .
Ho1 O4 C13 C14 1.0(11) .
Ho1 O4 C13 C16 -176.7(4) .
O4 C13 C14 C15 4.5(11) .
C16 C13 C14 C15 -177.8(7) .
Ho1 O5 C15 C14 -18.5(12) .
Ho1 O5 C15 C17 160.8(5) .
C13 C14 C15 O5 3.4(11) .
C13 C14 C15 C17 -176.0(7) .
