#------------------------------------------------------------------------------
#$Date: 2018-01-01 00:12:59 +0200 (Mon, 01 Jan 2018) $
#$Revision: 204627 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/43/4514330.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_4514330
loop_
_publ_author_name
'Angeli, Giasemi K.'
'Sartsidou, Christina'
'Vlachaki, Styliani'
'Spanopoulos, Ioannis'
'Tsangarakis, Constantinos'
'Kourtellaris, Andreas'
'Klontzas, Emmanuel'
'Froudakis, George E.'
'Tasiopoulos, Anastasios'
'Trikalitis, Pantelis N.'
_publ_section_title
;
 Reticular Chemistry and the Discovery of a New Family of Rare Earth (4,
 8)-Connected Metal-Organic Frameworks with csq Topology Based on
 RE4(μ3-O)2(COO)8 Clusters.
;
_journal_issue                   51
_journal_name_full               'ACS applied materials & interfaces'
_journal_page_first              44560
_journal_page_last               44566
_journal_paper_doi               10.1021/acsami.7b16380
_journal_volume                  9
_journal_year                    2017
_chemical_formula_moiety         'C39 H29 Ho2 N O12'
_chemical_formula_sum            'C39 H29 Ho2 N O12'
_chemical_formula_weight         1033.49
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_symmetry_space_group_name_Hall  '-P 6 2'
_symmetry_space_group_name_H-M   'P 6/m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   26.5159(7)
_cell_length_b                   26.5159(7)
_cell_length_c                   16.5671(6)
_cell_measurement_reflns_used    6839
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.4070
_cell_measurement_theta_min      5.7460
_cell_volume                     10087.6(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4223
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24535
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.980
_diffrn_reflns_theta_min         3.289
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.565
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.021
_exptl_crystal_description       cube
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.804
_refine_diff_density_min         -2.182
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.492
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         3649
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.499
_refine_ls_R_factor_all          0.1307
_refine_ls_R_factor_gt           0.1161
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3540
_refine_ls_wR_factor_ref         0.3866
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2440
_reflns_number_total             3649
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            am7b16380_si_003.cif
_cod_data_source_block           '_Ho_5_cu_sq'
_cod_original_cell_volume        10087.6(6)
_cod_database_code               4514330
_shelx_shelxl_version_number     2014/7
_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.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.452
_oxdiff_exptl_absorpt_empirical_full_max 1.548
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z'
'-x+y, y, -z'
'x, x-y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, z'
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
Ho1 Ho 0.45867(2) 0.54133(2) 0.5000 0.1441(6) Uani 1 4 d S T P
Ho2 Ho 0.63452(5) 0.63452(5) 0.5000 0.1455(6) Uani 1 4 d S T P
O3 O 0.5481(3) 0.5481(3) 0.5000 0.115(2) Uani 1 4 d S T P
C1 C 0.5281(7) 0.7109(5) 1.0000 0.153(4) Uani 1 2 d DS T P
O2 O 0.5904(7) 0.6535(6) 0.6028(8) 0.280(7) Uani 1 1 d . . .
C2 C 0.5285(5) 0.7388(4) 0.9277(5) 0.152(3) Uani 1 1 d D . .
O1 O 0.4958(7) 0.6077(5) 0.5902(7) 0.260(5) Uani 1 1 d . . .
C3 C 0.5264(12) 0.6536(7) 1.0000 0.215(9) Uani 1 2 d DS T P
H3A H 0.5263 0.6415 0.9454 0.323 Uiso 0.5 1 calc R U P
H3B H 0.5600 0.6575 1.0277 0.323 Uiso 0.5 1 calc R U P
H3C H 0.4917 0.6250 1.0269 0.323 Uiso 0.5 1 calc R U P
C4 C 0.5333(4) 0.7133(3) 0.8506(3) 0.158(3) Uani 1 1 d G . .
C5 C 0.4833(3) 0.6779(3) 0.8062(5) 0.201(5) Uani 1 1 d G . .
H5 H 0.4471 0.6700 0.8253 0.242 Uiso 1 1 calc R U .
C6 C 0.4875(4) 0.6545(3) 0.7332(5) 0.233(8) Uani 1 1 d G . .
H6 H 0.4541 0.6308 0.7035 0.280 Uiso 1 1 calc R U .
C7 C 0.5417(5) 0.6664(4) 0.7046(4) 0.220(7) Uani 1 1 d DG . .
C8 C 0.5916(4) 0.7017(4) 0.7490(5) 0.268(9) Uani 1 1 d G . .
H8 H 0.6278 0.7097 0.7299 0.322 Uiso 1 1 calc R U .
C9 C 0.5874(3) 0.7252(4) 0.8220(5) 0.214(6) Uani 1 1 d G . .
H9 H 0.6208 0.7489 0.8517 0.256 Uiso 1 1 calc R U .
C10 C 0.5433(9) 0.6386(8) 0.6264(8) 0.210(6) Uani 1 1 d D U .
N1 N 0.5000 0.5000 0.7700(7) 0.151(5) Uani 1 4 d DS T P
C11 C 0.5000 0.5000 0.6934(10) 0.221(13) Uani 1 4 d DS T P
H11 H 0.5182 0.4818 0.6690 0.265 Uiso 0.5 2 calc R U P
O6 O 0.4795(4) 0.5205(4) 0.6483(10) 0.176(6) Uani 0.5 2 d DS TU P
C12 C 0.5430(9) 0.5430(9) 0.811(2) 0.357(19) Uani 1 2 d DS TU P
H12A H 0.5358 0.5358 0.8680 0.535 Uiso 1 2 calc R U P
H12B H 0.5792 0.5450 0.7977 0.535 Uiso 0.5 1 calc R U P
H12C H 0.5450 0.5792 0.7977 0.535 Uiso 0.5 1 calc R U P
O5 O 0.7329(8) 0.6909(15) 0.5000 0.265(16) Uani 0.5 2 d S T P
O4 O 0.4370(9) 0.6200(10) 0.5000 0.224(11) Uani 0.5 2 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -14.9734 3.7046 '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 O1 88.7(8) 10_666 19_665
O1 Ho1 O1 80.0(9) 10_666 16_556
O1 Ho1 O1 143.4(7) 19_665 16_556
O1 Ho1 O1 143.4(7) 10_666 .
O1 Ho1 O1 80.0(9) 19_665 .
O1 Ho1 O1 88.7(8) 16_556 .
O1 Ho1 O3 128.2(4) 10_666 .
O1 Ho1 O3 128.2(4) 19_665 .
O1 Ho1 O3 84.4(4) 16_556 .
O1 Ho1 O3 84.4(4) . .
O1 Ho1 O3 84.4(4) 10_666 13_666
O1 Ho1 O3 84.4(4) 19_665 13_666
O1 Ho1 O3 128.2(4) 16_556 13_666
O1 Ho1 O3 128.2(4) . 13_666
O3 Ho1 O3 67.8(3) . 13_666
O1 Ho1 O4 84.4(6) 10_666 .
O1 Ho1 O4 84.4(6) 19_665 .
O1 Ho1 O4 60.1(5) 16_556 .
O1 Ho1 O4 60.1(5) . .
O3 Ho1 O4 128.0(5) . .
O3 Ho1 O4 164.3(5) 13_666 .
O1 Ho1 O4 60.1(5) 10_666 19_665
O1 Ho1 O4 60.1(5) 19_665 19_665
O1 Ho1 O4 84.4(6) 16_556 19_665
O1 Ho1 O4 84.4(6) . 19_665
O3 Ho1 O4 164.3(5) . 19_665
O3 Ho1 O4 127.9(5) 13_666 19_665
O4 Ho1 O4 36.3(10) . 19_665
O1 Ho1 O6 57.5(5) 10_666 16_556
O1 Ho1 O6 139.9(5) 19_665 16_556
O1 Ho1 O6 57.5(5) 16_556 16_556
O1 Ho1 O6 139.9(5) . 16_556
O3 Ho1 O6 72.5(4) . 16_556
O3 Ho1 O6 72.5(4) 13_666 16_556
O4 Ho1 O6 110.1(4) . 16_556
O4 Ho1 O6 110.1(4) 19_665 16_556
O1 Ho1 O6 139.9(4) 10_666 .
O1 Ho1 O6 57.5(5) 19_665 .
O1 Ho1 O6 139.9(5) 16_556 .
O1 Ho1 O6 57.5(5) . .
O3 Ho1 O6 72.5(4) . .
O3 Ho1 O6 72.5(4) 13_666 .
O4 Ho1 O6 110.1(4) . .
O4 Ho1 O6 110.1(4) 19_665 .
O6 Ho1 O6 137.5(9) 16_556 .
O1 Ho1 Ho1 108.3(4) 10_666 13_666
O1 Ho1 Ho1 108.3(4) 19_665 13_666
O1 Ho1 Ho1 108.3(4) 16_556 13_666
O1 Ho1 Ho1 108.3(4) . 13_666
O3 Ho1 Ho1 33.88(15) . 13_666
O3 Ho1 Ho1 33.88(15) 13_666 13_666
O4 Ho1 Ho1 161.8(5) . 13_666
O4 Ho1 Ho1 161.8(5) 19_665 13_666
O6 Ho1 Ho1 68.7(4) 16_556 13_666
O6 Ho1 Ho1 68.7(4) . 13_666
O2 Ho2 O2 79.7(9) 7_556 16_556
O2 Ho2 O2 97.8(9) 7_556 22
O2 Ho2 O2 163.0(7) 16_556 22
O2 Ho2 O2 163.0(7) 7_556 .
O2 Ho2 O2 97.8(9) 16_556 .
O2 Ho2 O2 79.7(9) 22 .
O2 Ho2 O5 114.0(6) 7_556 7_556
O2 Ho2 O5 82.0(8) 16_556 7_556
O2 Ho2 O5 114.0(6) 22 7_556
O2 Ho2 O5 82.0(8) . 7_556
O2 Ho2 O5 82.0(8) 7_556 .
O2 Ho2 O5 114.0(6) 16_556 .
O2 Ho2 O5 82.0(8) 22 .
O2 Ho2 O5 114.0(6) . .
O5 Ho2 O5 50.3(19) 7_556 .
O2 Ho2 O3 81.5(3) 7_556 .
O2 Ho2 O3 81.5(3) 16_556 .
O2 Ho2 O3 81.5(3) 22 .
O2 Ho2 O3 81.5(3) . .
O5 Ho2 O3 154.8(9) 7_556 .
O5 Ho2 O3 154.8(9) . .
Ho1 O3 Ho1 112.2(3) 13_666 .
Ho1 O3 Ho2 123.88(15) 13_666 .
Ho1 O3 Ho2 123.88(15) . .
C2 C1 C2 117.0(10) 16_557 .
C2 C1 C3 121.5(5) 16_557 .
C2 C1 C3 121.5(5) . .
C10 O2 Ho2 139.4(10) . .
C2 C2 C1 121.5(5) 21_565 .
C2 C2 C4 119.9(4) 21_565 .
C1 C2 C4 118.4(7) . .
C10 O1 Ho1 140.3(12) . .
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C5 C4 C9 120.0 . .
C5 C4 C2 119.7(7) . .
C9 C4 C2 120.3(7) . .
C4 C5 C6 120.0 . .
C4 C5 H5 120.0 . .
C6 C5 H5 120.0 . .
C7 C6 C5 120.0 . .
C7 C6 H6 120.0 . .
C5 C6 H6 120.0 . .
C6 C7 C8 120.0 . .
C6 C7 C10 117.5(11) . .
C8 C7 C10 122.5(11) . .
C7 C8 C9 120.0 . .
C7 C8 H8 120.0 . .
C9 C8 H8 120.0 . .
C8 C9 C4 120.0 . .
C8 C9 H9 120.0 . .
C4 C9 H9 120.0 . .
O2 C10 O1 127.5(12) . .
O2 C10 C7 114.1(16) . .
O1 C10 C7 117.9(16) . .
C11 N1 C12 120.9(19) . 4_665
C11 N1 C12 120.9(19) . .
C12 N1 C12 118(4) 4_665 .
O6 C11 N1 128.4(13) . .
O6 C11 H11 115.8 . .
N1 C11 H11 115.8 . .
C11 O6 Ho1 149.7(17) . .
N1 C12 H12A 109.5 . .
N1 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
N1 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
O4 O4 Ho1 71.8(5) 19_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ho1 O1 2.137(9) 10_666
Ho1 O1 2.137(9) 19_665
Ho1 O1 2.137(9) 16_556
Ho1 O1 2.137(9) .
Ho1 O3 2.286(4) .
Ho1 O3 2.286(4) 13_666
Ho1 O4 2.424(17) .
Ho1 O4 2.424(17) 19_665
Ho1 O6 2.636(13) 16_556
Ho1 O6 2.636(13) .
Ho1 Ho1 3.7962(18) 13_666
Ho2 O2 2.261(12) 7_556
Ho2 O2 2.261(12) 16_556
Ho2 O2 2.261(12) 22
Ho2 O2 2.262(12) .
Ho2 O5 2.27(2) 7_556
Ho2 O5 2.27(2) .
Ho2 O3 2.293(7) .
O3 Ho1 2.286(4) 13_666
C1 C2 1.404(7) 16_557
C1 C2 1.404(7) .
C1 C3 1.496(9) .
O2 C10 1.17(2) .
C2 C2 1.352(17) 21_565
C2 C4 1.480(10) .
O1 C10 1.26(2) .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 C5 1.3900 .
C4 C9 1.3900 .
C5 C6 1.3900 .
C5 H5 0.9300 .
C6 C7 1.3900 .
C6 H6 0.9300 .
C7 C8 1.3900 .
C7 C10 1.500(9) .
C8 C9 1.3900 .
C8 H8 0.9300 .
C9 H9 0.9300 .
N1 C11 1.27(2) .
N1 C12 1.328(10) 4_665
N1 C12 1.328(10) .
C11 O6 1.203(9) .
C11 H11 0.9300 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
O4 O4 1.51(5) 19_665
