#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:44:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179732 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/28/7002802.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_7002802
loop_
_publ_author_name
'Liu, Yen-Shen'
'Tang, Ming-Feng'
'Lii, Kwang-Hwa'
_publ_section_title
;
 Rare earth metal squarates incorporating ethylene glycol ligand with a
 three-dimensional framework structure: RE(C4O4)1.5(C2H6O2) (RE = Y,
 La--Nd, Sm--Lu)
;
_journal_issue                   44
_journal_name_full               'Dalton Transactions'
_journal_page_first              9781
_journal_page_last               9786
_journal_paper_doi               10.1039/b911962k
_journal_year                    2009
_chemical_formula_moiety         Ho(C4O4)1.5(C2H6O2)
_chemical_formula_sum            'C8 H6 Ho O8'
_chemical_formula_weight         395.06
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.151(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.7571(5)
_cell_length_b                   12.0918(5)
_cell_length_c                   12.5485(5)
_cell_measurement_temperature    296(2)
_cell_volume                     1911.05(13)
_computing_cell_refinement       'Bruker SHELXTL'
_computing_data_collection       'Bruker SHELXTL'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9103
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    8.312
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5123
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.490
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0166
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0206P)²+4.4358P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0398
_refine_ls_wR_factor_ref         0.0404
_reflns_number_gt                2250
_reflns_number_total             2384
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b911962k.txt
_cod_data_source_block           HoSqEg
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7002802
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Ho1 Ho 0.272780(8) 0.463172(9) 0.222446(8) 0.01071(5) Uani 1 1 d . . .
O1 O 0.23953(16) 0.40996(15) 0.40090(14) 0.0169(4) Uani 1 1 d . . .
O2 O 0.20915(16) 0.14688(15) 0.34579(14) 0.0187(4) Uani 1 1 d . . .
O3 O 0.37006(16) 0.43182(19) 0.08730(16) 0.0241(4) Uani 1 1 d . . .
O4 O 0.59882(16) 0.55203(17) 0.16074(15) 0.0201(4) Uani 1 1 d . . .
O5 O 0.37847(17) 0.31502(18) 0.27713(18) 0.0274(5) Uani 1 1 d . . .
O6 O 0.37476(18) 0.04992(17) 0.24225(19) 0.0263(5) Uani 1 1 d . . .
O7 O 0.14947(18) 0.46622(17) 0.04845(18) 0.0235(5) Uani 1 1 d . . .
O8 O 0.1586(2) 0.30796(19) 0.18966(19) 0.0327(5) Uani 1 1 d . . .
C1 C 0.2453(2) 0.3216(2) 0.45383(19) 0.0141(5) Uani 1 1 d . . .
C2 C 0.2325(2) 0.2031(2) 0.4302(2) 0.0145(5) Uani 1 1 d . . .
C3 C 0.4415(2) 0.4693(2) 0.0402(2) 0.0162(5) Uani 1 1 d . . .
C4 C 0.5443(2) 0.5224(2) 0.0729(2) 0.0145(5) Uani 1 1 d . . .
C5 C 0.4439(2) 0.2447(2) 0.2583(2) 0.0148(5) Uani 1 1 d . . .
C6 C 0.44319(19) 0.1245(2) 0.2506(2) 0.0138(5) Uani 1 1 d . . .
C7 C 0.0867(3) 0.3691(3) 0.0170(3) 0.0348(8) Uani 1 1 d . . .
C8 C 0.0602(3) 0.3194(3) 0.1177(3) 0.0341(8) Uani 1 1 d . . .
H7A H 0.131(4) 0.308(5) -0.017(4) 0.091(18) Uiso 1 1 d . . .
H7B H 0.019(3) 0.387(3) -0.029(3) 0.037(10) Uiso 1 1 d . . .
H8A H 0.019(3) 0.246(3) 0.098(3) 0.036(10) Uiso 1 1 d . . .
H8B H 0.009(3) 0.375(3) 0.150(3) 0.039(11) Uiso 1 1 d . . .
H8O H 0.164(3) 0.252(3) 0.222(3) 0.037(11) Uiso 1 1 d . . .
H7O H 0.184(4) 0.483(3) 0.001(4) 0.041(12) Uiso 1 1 d . . .
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'
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
_geom_angle_publ_flag
O6 Ho1 O5 140.95(8) 4 . ?
O6 Ho1 O4 100.98(8) 4 2_655 ?
O5 Ho1 O4 81.21(8) . 2_655 ?
O6 Ho1 O3 142.16(8) 4 . ?
O5 Ho1 O3 74.24(8) . . ?
O4 Ho1 O3 97.79(8) 2_655 . ?
O6 Ho1 O8 83.88(9) 4 . ?
O5 Ho1 O8 75.41(9) . . ?
O4 Ho1 O8 147.28(7) 2_655 . ?
O3 Ho1 O8 97.53(9) . . ?
O6 Ho1 O2 76.76(7) 4 4 ?
O5 Ho1 O2 138.32(7) . 4 ?
O4 Ho1 O2 72.22(7) 2_655 4 ?
O3 Ho1 O2 78.17(7) . 4 ?
O8 Ho1 O2 139.49(7) . 4 ?
O6 Ho1 O1 70.70(7) 4 . ?
O5 Ho1 O1 72.33(7) . . ?
O4 Ho1 O1 75.28(7) 2_655 . ?
O3 Ho1 O1 146.51(7) . . ?
O8 Ho1 O1 75.99(7) . . ?
O2 Ho1 O1 127.81(6) 4 . ?
O6 Ho1 O7 74.59(8) 4 . ?
O5 Ho1 O7 122.57(8) . . ?
O4 Ho1 O7 147.92(7) 2_655 . ?
O3 Ho1 O7 72.10(8) . . ?
O8 Ho1 O7 64.71(7) . . ?
O2 Ho1 O7 75.88(6) 4 . ?
O1 Ho1 O7 129.47(7) . . ?
C1 O1 Ho1 135.17(16) . . ?
C2 O2 Ho1 141.10(17) . 4_545 ?
C3 O3 Ho1 144.5(2) . . ?
C4 O4 Ho1 131.92(17) . 2_655 ?
C5 O5 Ho1 149.82(19) . . ?
C6 O6 Ho1 155.88(19) . 4_545 ?
C7 O7 Ho1 118.45(18) . . ?
C7 O7 H7O 110(3) . . ?
Ho1 O7 H7O 108(3) . . ?
C8 O8 Ho1 119.09(19) . . ?
C8 O8 H8O 114(3) . . ?
Ho1 O8 H8O 126(3) . . ?
O1 C1 C2 136.9(2) . . ?
O1 C1 C2 133.2(2) . 7_556 ?
C2 C1 C2 90.0(2) . 7_556 ?
O2 C2 C1 134.8(2) . . ?
O2 C2 C1 135.2(2) . 7_556 ?
C1 C2 C1 90.0(2) . 7_556 ?
O3 C3 C4 136.0(3) . . ?
O3 C3 C4 134.1(3) . 5_665 ?
C4 C3 C4 89.9(2) . 5_665 ?
O4 C4 C3 135.9(3) . . ?
O4 C4 C3 134.0(3) . 5_665 ?
C3 C4 C3 90.1(2) . 5_665 ?
O5 C5 C6 134.4(2) . . ?
O5 C5 C5 136.28(16) . 2_655 ?
C6 C5 C5 89.25(14) . 2_655 ?
O6 C6 C6 133.27(16) . 2_655 ?
O6 C6 C5 136.4(2) . . ?
C6 C6 C5 90.26(14) 2_655 . ?
O7 C7 C8 106.8(3) . . ?
O7 C7 H7A 112(3) . . ?
C8 C7 H7A 105(3) . . ?
O7 C7 H7B 113(2) . . ?
C8 C7 H7B 107(2) . . ?
H7A C7 H7B 113(4) . . ?
O8 C8 C7 106.3(3) . . ?
O8 C8 H8A 115(2) . . ?
C7 C8 H8A 109(2) . . ?
O8 C8 H8B 111(2) . . ?
C7 C8 H8B 108(2) . . ?
H8A C8 H8B 108(3) . . ?
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
Ho1 O6 2.259(2) 4 ?
Ho1 O5 2.281(2) . ?
Ho1 O4 2.2852(19) 2_655 ?
Ho1 O3 2.2867(19) . ?
Ho1 O8 2.372(2) . ?
Ho1 O2 2.4049(18) 4 ?
Ho1 O1 2.4311(17) . ?
Ho1 O7 2.480(2) . ?
O1 C1 1.254(3) . ?
O2 C2 1.254(3) . ?
O2 Ho1 2.4049(18) 4_545 ?
O3 C3 1.248(3) . ?
O4 C4 1.258(3) . ?
O4 Ho1 2.2852(19) 2_655 ?
O5 C5 1.241(3) . ?
O6 C6 1.248(3) . ?
O6 Ho1 2.259(2) 4_545 ?
O7 C7 1.441(4) . ?
O7 H7O 0.82(4) . ?
O8 C8 1.432(4) . ?
O8 H8O 0.79(4) . ?
C1 C2 1.467(4) . ?
C1 C2 1.469(3) 7_556 ?
C2 C1 1.469(3) 7_556 ?
C3 C4 1.459(4) . ?
C3 C4 1.462(4) 5_665 ?
C4 C3 1.462(4) 5_665 ?
C5 C6 1.456(4) . ?
C5 C5 1.477(5) 2_655 ?
C6 C6 1.452(5) 2_655 ?
C7 C8 1.487(5) . ?
C7 H7A 1.05(6) . ?
C7 H7B 0.98(4) . ?
C8 H8A 1.05(4) . ?
C8 H8B 1.07(4) . ?
