#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:46:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179127 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/89/4308904.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_4308904
loop_
_publ_author_name
'Xiaodan Guo'
'Guangshan Zhu'
'Qianrong Fang'
'Ming Xue'
'Ge Tian'
'Jinyu Sun'
'Xiaotian Li'
'Shilun Qiu'
_publ_section_title
;
Synthesis, Structure and Luminescent Properties of Rare Earth Coordination
Polymers Constructed from Paddle-Wheel Building Blocks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3850
_journal_page_last               3855
_journal_paper_doi               10.1021/ic0500457
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C21 H14 Ho N0 O7'
_chemical_formula_weight         543.25
_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                 106.887(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.2219(14)
_cell_length_b                   17.0779(14)
_cell_length_c                   18.5141(12)
_cell_measurement_temperature    273(2)
_cell_volume                     7630.8(9)
_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      273(2)
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_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  0.1151
_diffrn_reflns_av_sigmaI/netI    0.1504
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22402
_diffrn_reflns_theta_full        28.19
_diffrn_reflns_theta_max         28.19
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.094
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.946
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.834
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         8405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0613
_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)+(0.0553P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1490
_reflns_number_gt                4838
_reflns_number_total             8405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0500457si20050112_103555_2.cif
_cod_data_source_block           Ho(bpdc)1.5(H2O)
_cod_database_code               4308904
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 0.997249(14) 0.95909(2) 0.104337(19) 0.02978(12) Uani 1 1 d . . .
O1 O 0.9421(2) 0.9289(4) -0.0127(3) 0.0560(18) Uani 1 1 d . . .
O2 O 0.92866(19) 0.9679(3) 0.1610(3) 0.0442(14) Uani 1 1 d . . .
O3 O 1.0617(2) 0.8943(4) 0.0603(3) 0.0491(16) Uani 1 1 d . . .
O4 O 1.0523(2) 0.9282(4) 0.2209(3) 0.0540(17) Uani 1 1 d . . .
O5 O 1.0652(3) 1.0547(4) 0.1334(4) 0.0557(17) Uani 1 1 d . . .
O6 O 0.9511(2) 1.0734(3) 0.0595(3) 0.0458(15) Uani 1 1 d . . .
O7 N 0.9725(3) 0.8251(4) 0.1181(4) 0.0505(19) Uani 1 1 d . . .
C1 C 1.0793(4) 1.0870(5) 0.0804(5) 0.044(2) Uani 1 1 d . . .
C2 C 1.1258(3) 1.1433(5) 0.0997(5) 0.047(2) Uani 1 1 d . . .
C3 C 1.1505(5) 1.1676(7) 0.1754(5) 0.075(4) Uani 1 1 d . . .
H3A H 1.1362 1.1493 0.2132 0.080 Uiso 1 1 calc R . .
C4 C 1.1942(5) 1.2164(7) 0.1934(6) 0.080(4) Uani 1 1 d . . .
H4A H 1.2094 1.2302 0.2437 0.080 Uiso 1 1 calc R . .
C5 C 1.2175(4) 1.2473(6) 0.1406(5) 0.057(3) Uani 1 1 d . . .
C6 C 1.1911(4) 1.2250(7) 0.0665(5) 0.077(4) Uani 1 1 d . . .
H6A H 1.2044 1.2449 0.0283 0.080 Uiso 1 1 calc R . .
C7 C 1.1469(4) 1.1757(8) 0.0471(6) 0.079(4) Uani 1 1 d . . .
H7A H 1.1307 1.1638 -0.0035 0.080 Uiso 1 1 calc R . .
C8 C 0.9254(3) 1.1063(5) 0.0009(5) 0.0367(19) Uani 1 1 d . . .
C9 C 0.8740(4) 1.1495(5) 0.0021(5) 0.047(2) Uani 1 1 d . . .
C10 C 0.8492(5) 1.2031(9) -0.0544(7) 0.112(6) Uani 1 1 d . . .
H10A H 0.8649 1.2118 -0.0934 0.080 Uiso 1 1 calc R . .
C11 C 0.8019(5) 1.2434(7) -0.0538(6) 0.085(4) Uani 1 1 d . . .
H11A H 0.7872 1.2805 -0.0910 0.080 Uiso 1 1 calc R . .
C12 C 0.7763(4) 1.2294(6) 0.0010(5) 0.061(3) Uani 1 1 d . . .
C13 C 0.8027(5) 1.1784(7) 0.0575(6) 0.084(4) Uani 1 1 d . . .
H13A H 0.7879 1.1710 0.0976 0.080 Uiso 1 1 calc R . .
C14 C 0.8496(4) 1.1378(7) 0.0577(6) 0.078(4) Uani 1 1 d . . .
H14A H 0.8649 1.1021 0.0961 0.080 Uiso 1 1 calc R . .
C15 C 0.9172(3) 0.9331(4) 0.2142(5) 0.0320(18) Uani 1 1 d . . .
C16 C 0.8640(3) 0.8882(5) 0.1954(5) 0.040(2) Uani 1 1 d . . .
C17 C 0.8234(4) 0.8975(6) 0.1280(5) 0.063(3) Uani 1 1 d . . .
H17A H 0.8288 0.9337 0.0933 0.080 Uiso 1 1 calc R . .
C18 C 0.7750(4) 0.8548(6) 0.1102(5) 0.064(3) Uani 1 1 d . . .
H18A H 0.7480 0.8640 0.0647 0.080 Uiso 1 1 calc R . .
C19 C 0.7659(4) 0.7980(6) 0.1593(5) 0.053(3) Uani 1 1 d . . .
C20 C 0.8073(4) 0.7903(7) 0.2293(5) 0.071(3) Uani 1 1 d . . .
H20A H 0.8024 0.7540 0.2643 0.080 Uiso 1 1 calc R . .
C21 C 0.8536(4) 0.8341(6) 0.2466(5) 0.058(3) Uani 1 1 d . . .
H21A H 0.8793 0.8283 0.2937 0.080 Uiso 1 1 calc R . .
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
O4 Ho1 O1 153.4(2) . . ?
O4 Ho1 O2 85.0(2) . . ?
O1 Ho1 O2 96.8(2) . . ?
O4 Ho1 O6 130.4(2) . . ?
O1 Ho1 O6 75.1(2) . . ?
O2 Ho1 O6 74.8(2) . . ?
O4 Ho1 O3 85.7(2) . . ?
O1 Ho1 O3 81.5(2) . . ?
O2 Ho1 O3 154.8(2) . . ?
O6 Ho1 O3 128.0(2) . . ?
O4 Ho1 O5 74.6(2) . . ?
O1 Ho1 O5 126.1(2) . . ?
O2 Ho1 O5 117.2(2) . . ?
O6 Ho1 O5 75.4(2) . . ?
O3 Ho1 O5 82.6(2) . . ?
O4 Ho1 O7 77.5(2) . . ?
O1 Ho1 O7 77.2(3) . . ?
O2 Ho1 O7 76.0(2) . . ?
O6 Ho1 O7 136.5(2) . . ?
O3 Ho1 O7 79.1(2) . . ?
O5 Ho1 O7 147.6(2) . . ?
C1 O1 Ho1 168.4(6) 5_775 . ?
C15 O2 Ho1 135.3(5) . . ?
C8 O3 Ho1 135.4(5) 5_775 . ?
C15 O4 Ho1 162.7(6) 2_755 . ?
C1 O5 Ho1 119.0(5) . . ?
C8 O6 Ho1 142.2(5) . . ?
O1 C1 O5 123.3(8) 5_775 . ?
O1 C1 C2 117.9(9) 5_775 . ?
O5 C1 C2 118.7(8) . . ?
C7 C2 C3 116.0(8) . . ?
C7 C2 C1 122.8(8) . . ?
C3 C2 C1 121.2(8) . . ?
C4 C3 C2 121.2(9) . . ?
C3 C4 C5 123.2(9) . . ?
C4 C5 C6 114.3(8) . . ?
C4 C5 C19 124.0(8) . 3 ?
C6 C5 C19 121.7(8) . 3 ?
C7 C6 C5 123.4(9) . . ?
C2 C7 C6 121.7(9) . . ?
O6 C8 O3 125.4(7) . 5_775 ?
O6 C8 C9 116.7(7) . . ?
O3 C8 C9 117.8(7) 5_775 . ?
C14 C9 C10 117.5(8) . . ?
C14 C9 C8 121.6(8) . . ?
C10 C9 C8 121.0(8) . . ?
C11 C10 C9 121.6(9) . . ?
C12 C11 C10 120.8(9) . . ?
C11 C12 C13 116.4(8) . . ?
C11 C12 C12 120.3(11) . 7_675 ?
C13 C12 C12 123.3(11) . 7_675 ?
C14 C13 C12 123.3(9) . . ?
C9 C14 C13 120.3(9) . . ?
O4 C15 O2 125.3(7) 2_755 . ?
O4 C15 C16 117.3(7) 2_755 . ?
O2 C15 C16 117.1(7) . . ?
C17 C16 C21 116.9(8) . . ?
C17 C16 C15 122.3(8) . . ?
C21 C16 C15 120.8(7) . . ?
C16 C17 C18 122.1(9) . . ?
C17 C18 C19 121.0(9) . . ?
C18 C19 C20 116.5(8) . . ?
C18 C19 C5 123.1(8) . 3_445 ?
C20 C19 C5 120.4(8) . 3_445 ?
C21 C20 C19 121.6(9) . . ?
C20 C21 C16 121.8(8) . . ?
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 O4 2.264(6) . ?
Ho1 O1 2.269(6) . ?
Ho1 O2 2.274(5) . ?
Ho1 O6 2.301(6) . ?
Ho1 O3 2.303(5) . ?
Ho1 O5 2.314(6) . ?
Ho1 O7 2.405(7) . ?
O1 C1 1.243(10) 5_775 ?
O2 C15 1.254(9) . ?
O3 C8 1.266(9) 5_775 ?
O4 C15 1.226(9) 2_755 ?
O5 C1 1.264(10) . ?
O6 C8 1.227(9) . ?
C1 O1 1.243(10) 5_775 ?
C1 C2 1.478(12) . ?
C2 C7 1.355(12) . ?
C2 C3 1.420(12) . ?
C3 C4 1.344(13) . ?
C4 C5 1.383(12) . ?
C5 C6 1.392(12) . ?
C5 C19 1.454(12) 3 ?
C6 C7 1.359(13) . ?
C8 O3 1.266(9) 5_775 ?
C8 C9 1.496(10) . ?
C9 C14 1.359(12) . ?
C9 C10 1.393(13) . ?
C10 C11 1.380(13) . ?
C11 C12 1.374(12) . ?
C12 C13 1.375(13) . ?
C12 C12 1.492(16) 7_675 ?
C13 C14 1.371(12) . ?
C15 O4 1.226(9) 2_755 ?
C15 C16 1.494(10) . ?
C16 C17 1.375(12) . ?
C16 C21 1.402(11) . ?
C17 C18 1.377(12) . ?
C18 C19 1.393(12) . ?
C19 C20 1.415(12) . ?
C19 C5 1.454(12) 3_445 ?
C20 C21 1.344(12) . ?
