#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:24:52 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179109 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/71/4307146.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_4307146
loop_
_publ_author_name
'Zhongyue Li'
'Guangshan Zhu'
'Xiaodan Guo'
'Xiaojun Zhao'
'Zhao Jin'
'Shilun Qiu'
_publ_section_title
;
Synthesis, Structure, and Luminescent and Magnetic Properties of Novel
Lanthanide Metal-Organic Frameworks with Zeolite-like Topology
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5174
_journal_page_last               5178
_journal_paper_doi               10.1021/ic061666i
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C15 H19 Ho N2 O9'
_chemical_formula_weight         536.25
_chemical_name_common            Ho(BTC)(DMF)2(H2O)
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.06(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.440(4)
_cell_length_b                   11.647(2)
_cell_length_c                   19.698(4)
_cell_measurement_temperature    293(2)
_cell_volume                     4044.4(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.865
_diffrn_measured_fraction_theta_max 0.865
_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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10175
_diffrn_reflns_theta_full        27.75
_diffrn_reflns_theta_max         27.75
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.959
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.706
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4114
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          1.997
_refine_ls_shift/su_mean         0.046
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0706P)²+9.6244P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                3021
_reflns_number_total             4114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061666i-file001_3.cif
_cod_data_source_block           Ho(BTC)(DMF)2(H2O)
_cod_original_cell_volume        4044.5(14)
_cod_database_code               4307146
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 0.074964(17) 0.32957(3) 1.083162(16) 0.02253(13) Uani 1 1 d . . .
C1 C 0.1918(4) 0.1743(6) 1.1083(4) 0.0293(17) Uani 1 1 d . . .
C2 C 0.1243(4) 0.4213(6) 1.2175(4) 0.0268(16) Uani 1 1 d . . .
C3 C 0.0900(4) 0.5040(6) 0.9562(4) 0.0255(15) Uani 1 1 d . . .
C4 C 0.1337(4) 0.4887(6) 0.9055(4) 0.0257(15) Uani 1 1 d . . .
C5 C 0.1119(4) 0.5415(6) 0.8390(4) 0.0277(16) Uani 1 1 d . . .
H5 H 0.0691 0.5883 0.8269 0.033 Uiso 1 1 calc R . .
C6 C 0.1527(4) 0.5256(5) 0.7899(4) 0.0249(15) Uani 1 1 d . . .
C7 C 0.2161(4) 0.4580(6) 0.8083(4) 0.0304(16) Uani 1 1 d . . .
H7A H 0.2437 0.4474 0.7762 0.036 Uiso 1 1 calc R . .
C8 C 0.2400(4) 0.4049(6) 0.8744(4) 0.0262(15) Uani 1 1 d . . .
C9 C 0.1995(4) 0.4196(5) 0.9230(4) 0.0256(15) Uani 1 1 d . . .
H9 H 0.2156 0.3840 0.9671 0.031 Uiso 1 1 calc R . .
C10 C -0.0479(6) 0.2789(8) 0.9247(5) 0.049(2) Uani 1 1 d . . .
H10 H -0.0686 0.3523 0.9175 0.059 Uiso 1 1 calc R . .
C11 C -0.0618(9) 0.0800(10) 0.9025(8) 0.106(5) Uani 1 1 d . . .
H11A H -0.0266 0.0739 0.9492 0.159 Uiso 1 1 calc R . .
H11B H -0.0372 0.0571 0.8679 0.159 Uiso 1 1 calc R . .
H11C H -0.1045 0.0309 0.8991 0.159 Uiso 1 1 calc R . .
C12 C -0.1625(7) 0.2174(14) 0.8423(8) 0.126(7) Uani 1 1 d . . .
H12A H -0.1959 0.1569 0.8473 0.189 Uiso 1 1 calc R . .
H12B H -0.1606 0.2198 0.7941 0.189 Uiso 1 1 calc R . .
H12C H -0.1809 0.2895 0.8542 0.189 Uiso 1 1 calc R . .
C13 C -0.0508(6) 0.1793(7) 1.1316(5) 0.046(2) Uani 1 1 d . . .
H13 H -0.0232 0.1958 1.1782 0.055 Uiso 1 1 calc R . .
C14 C -0.1563(8) 0.1195(12) 1.1807(8) 0.096(4) Uani 1 1 d . . .
H14A H -0.1257 0.1559 1.2232 0.144 Uiso 1 1 calc R . .
H14B H -0.1594 0.0387 1.1889 0.144 Uiso 1 1 calc R . .
H14C H -0.2063 0.1522 1.1674 0.144 Uiso 1 1 calc R . .
C15 C -0.1629(12) 0.107(2) 1.0492(12) 0.228(12) Uani 1 1 d U . .
H15A H -0.1419 0.1475 1.0169 0.342 Uiso 1 1 calc R . .
H15B H -0.2154 0.1275 1.0400 0.342 Uiso 1 1 calc R . .
H15C H -0.1589 0.0259 1.0427 0.342 Uiso 1 1 calc R . .
N1 N -0.0870(5) 0.1962(7) 0.8896(5) 0.064(3) Uani 1 1 d . . .
N2 N -0.1212(5) 0.1379(8) 1.1225(5) 0.068(3) Uani 1 1 d . . .
O1 O 0.1748(4) 0.2309(6) 1.0526(3) 0.060(2) Uani 1 1 d . . .
O2 O 0.1538(4) 0.1806(5) 1.1508(4) 0.059(2) Uani 1 1 d . . .
O3 O 0.1553(3) 0.4491(5) 1.1708(3) 0.0451(15) Uani 1 1 d . . .
O4 O 0.0703(3) 0.3525(4) 1.2035(3) 0.0274(11) Uani 1 1 d . . .
O5 O -0.0267(3) 0.4464(5) 1.0663(3) 0.0439(15) Uani 1 1 d . . .
O6 O 0.1161(3) 0.4667(4) 1.0182(2) 0.0309(12) Uani 1 1 d . . .
O7 O 0.0159(4) 0.2673(6) 0.9677(3) 0.0539(17) Uani 1 1 d . . .
H7 H 0.0479 0.2232 0.9495 0.065 Uiso 1 1 calc R . .
O8 O -0.0197(4) 0.1974(5) 1.0884(3) 0.0498(16) Uani 1 1 d . . .
O1W O -0.006(4) 0.899(3) 0.237(3) 0.088(12) Uani 0.25 1 d PU . .
O2W O 0.0000 0.687(2) 0.2500 0.108(9) Uani 0.50 2 d SPU . .
O3W O 0.0196(13) 0.7958(17) 0.2650(13) 0.041(6) Uani 0.25 1 d PU . .
O4W O 0.0000 0.9883(12) 0.2500 0.058(6) Uani 0.50 2 d SP . .
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
_geom_angle_publ_flag
O5 Ho1 O6 84.01(19) . . ?
O5 Ho1 O7 85.1(2) . . ?
O6 Ho1 O7 79.0(2) . . ?
O5 Ho1 O8 78.8(2) . . ?
O6 Ho1 O8 147.7(2) . . ?
O7 Ho1 O8 72.5(2) . . ?
O5 Ho1 O3 93.9(2) . . ?
O6 Ho1 O3 76.12(19) . . ?
O7 Ho1 O3 155.1(2) . . ?
O8 Ho1 O3 131.8(2) . . ?
O5 Ho1 O1 156.7(2) . . ?
O6 Ho1 O1 77.9(2) . . ?
O7 Ho1 O1 77.2(2) . . ?
O8 Ho1 O1 109.4(3) . . ?
O3 Ho1 O1 95.9(3) . . ?
O5 Ho1 O2 149.0(2) . . ?
O6 Ho1 O2 124.3(2) . . ?
O7 Ho1 O2 110.5(2) . . ?
O8 Ho1 O2 80.7(3) . . ?
O3 Ho1 O2 82.7(3) . . ?
O1 Ho1 O2 53.6(2) . . ?
O5 Ho1 O4 79.07(19) . . ?
O6 Ho1 O4 125.47(17) . . ?
O7 Ho1 O4 148.5(2) . . ?
O8 Ho1 O4 77.77(19) . . ?
O3 Ho1 O4 54.14(18) . . ?
O1 Ho1 O4 123.55(19) . . ?
O2 Ho1 O4 74.0(2) . . ?
O5 Ho1 C1 175.1(2) . . ?
O6 Ho1 C1 100.8(2) . . ?
O7 Ho1 C1 95.1(2) . . ?
O8 Ho1 C1 96.6(2) . . ?
O3 Ho1 C1 88.0(2) . . ?
O1 Ho1 C1 26.8(2) . . ?
O2 Ho1 C1 26.9(2) . . ?
O4 Ho1 C1 98.5(2) . . ?
O5 Ho1 C2 86.2(2) . . ?
O6 Ho1 C2 101.25(19) . . ?
O7 Ho1 C2 171.1(2) . . ?
O8 Ho1 C2 104.6(2) . . ?
O3 Ho1 C2 27.3(2) . . ?
O1 Ho1 C2 111.6(2) . . ?
O2 Ho1 C2 76.8(2) . . ?
O4 Ho1 C2 26.89(19) . . ?
C1 Ho1 C2 93.5(2) . . ?
O1 C1 O2 121.4(7) . . ?
O1 C1 C8 120.0(7) . 7_557 ?
O2 C1 C8 118.7(7) . 7_557 ?
O1 C1 Ho1 60.6(4) . . ?
O2 C1 Ho1 61.0(4) . . ?
C8 C1 Ho1 175.9(5) 7_557 . ?
O4 C2 O3 120.5(7) . . ?
O4 C2 C6 120.7(7) . 6_566 ?
O3 C2 C6 118.8(6) . 6_566 ?
O4 C2 Ho1 61.3(4) . . ?
O3 C2 Ho1 59.3(4) . . ?
C6 C2 Ho1 178.0(5) 6_566 . ?
O6 C3 O5 123.6(7) . 5_567 ?
O6 C3 C4 119.4(6) . . ?
O5 C3 C4 117.0(6) 5_567 . ?
C5 C4 C9 118.1(7) . . ?
C5 C4 C3 121.3(6) . . ?
C9 C4 C3 120.5(6) . . ?
C4 C5 C6 121.6(6) . . ?
C7 C6 C5 118.9(6) . . ?
C7 C6 C2 121.5(7) . 6_565 ?
C5 C6 C2 119.5(6) . 6_565 ?
C6 C7 C8 121.0(7) . . ?
C9 C8 C7 120.3(6) . . ?
C9 C8 C1 120.0(6) . 7_557 ?
C7 C8 C1 119.6(7) . 7_557 ?
C8 C9 C4 120.0(6) . . ?
O7 C10 N1 124.0(9) . . ?
O8 C13 N2 128.6(10) . . ?
C10 N1 C11 121.0(10) . . ?
C10 N1 C12 120.1(10) . . ?
C11 N1 C12 118.5(10) . . ?
C13 N2 C15 115.2(13) . . ?
C13 N2 C14 124.7(10) . . ?
C15 N2 C14 120.1(14) . . ?
C1 O1 Ho1 92.6(5) . . ?
C1 O2 Ho1 92.2(4) . . ?
C2 O3 Ho1 93.5(4) . . ?
C2 O4 Ho1 91.9(4) . . ?
C3 O5 Ho1 165.9(5) 5_567 . ?
C3 O6 Ho1 133.3(5) . . ?
C10 O7 Ho1 135.4(6) . . ?
C13 O8 Ho1 132.5(6) . . ?
O1W O1W O4W 76(3) 2 . ?
O1W O1W O3W 93(4) 2 2 ?
O4W O1W O3W 164(6) . 2 ?
O1W O1W O3W 65(4) 2 . ?
O4W O1W O3W 140(5) . . ?
O3W O1W O3W 35(2) 2 . ?
O3W O2W O3W 34.7(19) 2 . ?
O3W O3W O1W 81(3) 2 2 ?
O3W O3W O1W 64(3) 2 . ?
O1W O3W O1W 22(4) 2 . ?
O3W O3W O2W 72.7(9) 2 . ?
O1W O3W O2W 152(3) 2 . ?
O1W O3W O2W 136(3) . . ?
O1W O4W O1W 27(5) . 2 ?
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 O5 2.261(5) . ?
Ho1 O6 2.309(5) . ?
Ho1 O7 2.331(6) . ?
Ho1 O8 2.352(6) . ?
Ho1 O3 2.369(5) . ?
Ho1 O1 2.393(6) . ?
Ho1 O2 2.401(5) . ?
Ho1 O4 2.412(5) . ?
Ho1 C1 2.744(7) . ?
Ho1 C2 2.750(7) . ?
C1 O1 1.240(9) . ?
C1 O2 1.241(10) . ?
C1 C8 1.516(9) 7_557 ?
C2 O4 1.244(8) . ?
C2 O3 1.262(9) . ?
C2 C6 1.500(9) 6_566 ?
C3 O6 1.253(8) . ?
C3 O5 1.260(8) 5_567 ?
C3 C4 1.467(10) . ?
C4 C5 1.396(10) . ?
C4 C9 1.411(9) . ?
C5 C6 1.401(10) . ?
C6 C7 1.367(9) . ?
C6 C2 1.500(9) 6_565 ?
C7 C8 1.391(10) . ?
C8 C9 1.386(10) . ?
C8 C1 1.516(9) 7_557 ?
C10 O7 1.238(11) . ?
C10 N1 1.278(11) . ?
C11 N1 1.429(13) . ?
C12 N1 1.451(15) . ?
C13 O8 1.176(11) . ?
C13 N2 1.345(13) . ?
C14 N2 1.487(15) . ?
C15 N2 1.47(2) . ?
O5 C3 1.260(8) 5_567 ?
O1W O1W 0.51(10) 2 ?
O1W O4W 1.07(3) . ?
O1W O3W 1.23(4) 2 ?
O1W O3W 1.35(4) . ?
O2W O3W 1.32(3) 2 ?
O2W O3W 1.32(3) . ?
O3W O3W 0.79(4) 2 ?
O3W O1W 1.23(4) 2 ?
O4W O1W 1.07(3) 2 ?
