#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:42:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179760 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/56/7005622.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_7005622
loop_
_publ_author_name
'Lipstman, Sophia'
'Muniappan, Sankar'
'George, Sumod'
'Goldberg, Israel'
_publ_section_title
;
 Framework coordination polymers of tetra(4-carboxyphenyl)porphyrin and
 lanthanide ions in crystalline solids.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3273
_journal_page_last               3281
_journal_paper_doi               10.1039/b703698a
_journal_year                    2007
_chemical_formula_moiety         'C48 H31 Dy N4 O10'
_chemical_formula_sum            'C48 H31 Dy N4 O10'
_chemical_formula_weight         986.27
_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                 99.6484(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.8851(5)
_cell_length_b                   26.4514(7)
_cell_length_c                   9.39160(10)
_cell_measurement_reflns_used    6039
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      1.41
_cell_volume                     5114.91(19)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        'Denzo & Scalepack'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. Phi & 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  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25563
_diffrn_reflns_theta_full        28.17
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         1.98
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.515
_exptl_absorpt_correction_T_max  0.8632
_exptl_absorpt_correction_T_min  0.5824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.839
_refine_diff_density_min         -1.900
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         6176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0524P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0811
_reflns_number_gt                5624
_reflns_number_total             6176
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b703698a.txt
_cod_data_source_block           Compound-1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7005622
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
Dy Dy 0.5000 0.506357(6) 0.7500 0.01092(6) Uani 1 2 d S . .
C1 C 0.5000 0.18236(12) 0.7500 0.0138(6) Uani 1 2 d S . .
C2 C 0.44734(12) 0.15818(9) 0.7953(3) 0.0157(5) Uani 1 1 d . . .
C3 C 0.39121(12) 0.18345(9) 0.8334(3) 0.0186(5) Uani 1 1 d . . .
H3 H 0.3828 0.2188 0.8286 0.022 Uiso 1 1 calc R . .
C4 C 0.35300(12) 0.14738(10) 0.8771(3) 0.0179(5) Uani 1 1 d . . .
H4 H 0.3125 0.1526 0.9081 0.022 Uiso 1 1 calc R . .
C5 C 0.38517(11) 0.09949(9) 0.8678(2) 0.0138(4) Uani 1 1 d . . .
C6 C 0.36544(11) 0.05317(9) 0.9178(2) 0.0135(5) Uani 1 1 d . . .
C7 C 0.39875(12) 0.00685(9) 0.9124(3) 0.0121(5) Uani 1 1 d . . .
C8 C 0.38356(12) -0.04028(9) 0.9755(3) 0.0167(5) Uani 1 1 d . . .
H8 H 0.3524 -0.0453 1.0372 0.020 Uiso 1 1 calc R . .
C9 C 0.42188(12) -0.07635(9) 0.9304(2) 0.0168(5) Uani 1 1 d . . .
H9 H 0.4232 -0.1111 0.9566 0.020 Uiso 1 1 calc R . .
C10 C 0.46036(11) -0.05227(9) 0.8354(2) 0.0138(4) Uani 1 1 d . . .
C11 C 0.5000 -0.07744(12) 0.7500 0.0143(6) Uani 1 2 d S . .
N12 N 0.44153(9) 0.10727(7) 0.8146(2) 0.0141(4) Uani 1 1 d . . .
H12 H 0.4689 0.0838 0.7961 0.017 Uiso 0.50 1 calc PR . .
N13 N 0.44704(11) -0.00134(7) 0.8325(2) 0.0127(4) Uani 1 1 d . . .
H13 H 0.4661 0.0219 0.7872 0.015 Uiso 0.50 1 calc PR . .
C14 C 0.5000 0.23856(13) 0.7500 0.0141(6) Uani 1 2 d S . .
C15 C 0.51593(17) 0.26511(11) 0.8769(3) 0.0361(8) Uani 1 1 d . . .
H15 H 0.5267 0.2473 0.9656 0.043 Uiso 1 1 calc R . .
C16 C 0.51643(17) 0.31739(11) 0.8770(3) 0.0366(8) Uani 1 1 d . . .
H16 H 0.5282 0.3352 0.9654 0.044 Uiso 1 1 calc R . .
C17 C 0.5000 0.34383(13) 0.7500 0.0162(7) Uani 1 2 d S . .
C18 C 0.5000 0.40023(13) 0.7500 0.0147(7) Uani 1 2 d S . .
O19 O 0.52158(8) 0.42385(6) 0.86508(16) 0.0150(3) Uani 1 1 d . . .
C20 C 0.30074(11) 0.05249(9) 0.9671(2) 0.0143(5) Uani 1 1 d . . .
C21 C 0.24569(11) 0.06300(9) 0.8652(2) 0.0148(5) Uani 1 1 d . . .
H21 H 0.2506 0.0737 0.7711 0.018 Uiso 1 1 calc R . .
C22 C 0.18389(11) 0.05804(9) 0.8990(2) 0.0152(5) Uani 1 1 d . . .
H22 H 0.1469 0.0650 0.8281 0.018 Uiso 1 1 calc R . .
C23 C 0.17609(11) 0.04282(9) 1.0372(2) 0.0126(4) Uani 1 1 d . . .
C24 C 0.23096(11) 0.03605(10) 1.1427(2) 0.0165(5) Uani 1 1 d . . .
H24 H 0.2261 0.0285 1.2392 0.020 Uiso 1 1 calc R . .
C25 C 0.29300(11) 0.04027(10) 1.1072(2) 0.0169(5) Uani 1 1 d . . .
H25 H 0.3301 0.0348 1.1791 0.020 Uiso 1 1 calc R . .
C26 C 0.10945(11) 0.02984(9) 1.0668(2) 0.0124(4) Uani 1 1 d . . .
O27 O 0.10185(8) 0.02256(7) 1.19595(17) 0.0152(3) Uani 1 1 d . . .
O28 O 0.06441(8) 0.02527(7) 0.96071(17) 0.0163(3) Uani 1 1 d . . .
C29 C 0.5000 -0.13349(12) 0.7500 0.0162(7) Uani 1 2 d S . .
C30 C 0.55767(12) -0.16095(10) 0.7864(3) 0.0197(5) Uani 1 1 d . . .
H30 H 0.5976 -0.1434 0.8123 0.024 Uiso 1 1 calc R . .
C31 C 0.55763(13) -0.21362(10) 0.7853(3) 0.0227(5) Uani 1 1 d . . .
H31 H 0.5976 -0.2313 0.8090 0.027 Uiso 1 1 calc R . .
C32 C 0.5000 -0.24078(14) 0.7500 0.0204(7) Uani 1 2 d S . .
C33 C 0.5000 -0.29814(14) 0.7500 0.0253(8) Uani 1 2 d S . .
O34 O 0.55367(11) -0.32054(7) 0.7571(2) 0.0348(5) Uani 1 1 d . . .
H34 H 0.5480 -0.3484 0.7210 0.052 Uiso 0.50 1 d P . .
O35 O 0.54910(8) 0.58088(6) 0.65790(17) 0.0158(3) Uani 1 1 d . . .
H35A H 0.5366 0.5824 0.5548 0.024 Uiso 1 1 d R . .
H35B H 0.5656 0.5517 0.6752 0.024 Uiso 1 1 d 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'
Dy Dy -0.1892 4.4098 '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
O28 Dy O28 154.36(9) 4_556 3 ?
O28 Dy O27 80.59(6) 4_556 7_557 ?
O28 Dy O27 107.79(6) 3 7_557 ?
O28 Dy O27 107.79(6) 4_556 8 ?
O28 Dy O27 80.58(6) 3 8 ?
O27 Dy O27 142.72(9) 7_557 8 ?
O28 Dy O35 84.71(6) 4_556 2_656 ?
O28 Dy O35 74.61(6) 3 2_656 ?
O27 Dy O35 75.08(6) 7_557 2_656 ?
O27 Dy O35 140.59(6) 8 2_656 ?
O28 Dy O35 74.61(6) 4_556 . ?
O28 Dy O35 84.71(6) 3 . ?
O27 Dy O35 140.60(6) 7_557 . ?
O27 Dy O35 75.08(6) 8 . ?
O35 Dy O35 72.60(8) 2_656 . ?
O28 Dy O19 128.69(6) 4_556 . ?
O28 Dy O19 76.78(6) 3 . ?
O27 Dy O19 74.05(6) 7_557 . ?
O27 Dy O19 72.77(6) 8 . ?
O35 Dy O19 128.36(5) 2_656 . ?
O35 Dy O19 144.99(6) . . ?
O28 Dy O19 76.78(6) 4_556 2_656 ?
O28 Dy O19 128.69(6) 3 2_656 ?
O27 Dy O19 72.77(6) 7_557 2_656 ?
O27 Dy O19 74.05(6) 8 2_656 ?
O35 Dy O19 144.99(6) 2_656 2_656 ?
O35 Dy O19 128.36(5) . 2_656 ?
O19 Dy O19 53.46(7) . 2_656 ?
O28 Dy C18 102.82(5) 4_556 . ?
O28 Dy C18 102.82(5) 3 . ?
O27 Dy C18 71.36(4) 7_557 . ?
O27 Dy C18 71.36(4) 8 . ?
O35 Dy C18 143.70(4) 2_656 . ?
O35 Dy C18 143.70(4) . . ?
O19 Dy C18 26.73(4) . . ?
O19 Dy C18 26.73(4) 2_656 . ?
O28 Dy H35B 84.4 4_556 . ?
O28 Dy H35B 80.5 3 . ?
O27 Dy H35B 159.4 7_557 . ?
O27 Dy H35B 56.0 8 . ?
O35 Dy H35B 89.6 2_656 . ?
O35 Dy H35B 19.2 . . ?
O19 Dy H35B 126.5 . . ?
O19 Dy H35B 117.3 2_656 . ?
C18 Dy H35B 126.2 . . ?
C2 C1 C2 125.6(3) . 2_656 ?
C2 C1 C14 117.21(15) . . ?
C2 C1 C14 117.21(15) 2_656 . ?
N12 C2 C1 125.6(2) . . ?
N12 C2 C3 109.2(2) . . ?
C1 C2 C3 125.1(2) . . ?
C4 C3 C2 107.1(2) . . ?
C4 C3 H3 126.5 . . ?
C2 C3 H3 126.5 . . ?
C3 C4 C5 107.3(2) . . ?
C3 C4 H4 126.4 . . ?
C5 C4 H4 126.4 . . ?
N12 C5 C6 125.0(2) . . ?
N12 C5 C4 109.1(2) . . ?
C6 C5 C4 125.6(2) . . ?
C5 C6 C7 124.9(2) . . ?
C5 C6 C20 116.4(2) . . ?
C7 C6 C20 118.3(2) . . ?
N13 C7 C6 124.6(2) . . ?
N13 C7 C8 108.8(2) . . ?
C6 C7 C8 126.3(2) . . ?
C9 C8 C7 107.4(2) . . ?
C9 C8 H8 126.3 . . ?
C7 C8 H8 126.3 . . ?
C8 C9 C10 107.5(2) . . ?
C8 C9 H9 126.3 . . ?
C10 C9 H9 126.3 . . ?
N13 C10 C11 125.9(2) . . ?
N13 C10 C9 108.2(2) . . ?
C11 C10 C9 125.6(2) . . ?
C10 C11 C10 123.7(3) . 2_656 ?
C10 C11 C29 118.13(15) . . ?
C10 C11 C29 118.13(15) 2_656 . ?
C2 N12 C5 107.28(19) . . ?
C2 N12 H12 126.4 . . ?
C5 N12 H12 126.4 . . ?
C7 N13 C10 107.97(19) . . ?
C7 N13 H13 126.0 . . ?
C10 N13 H13 126.0 . . ?
C15 C14 C15 118.6(3) 2_656 . ?
C15 C14 C1 120.69(17) 2_656 . ?
C15 C14 C1 120.69(17) . . ?
C14 C15 C16 120.8(3) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C17 C16 C15 120.5(3) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C16 118.9(3) . 2_656 ?
C16 C17 C18 120.56(17) . . ?
C16 C17 C18 120.56(17) 2_656 . ?
O19 C18 O19 120.8(3) 2_656 . ?
O19 C18 C17 119.62(15) 2_656 . ?
O19 C18 C17 119.62(15) . . ?
O19 C18 Dy 60.38(15) 2_656 . ?
O19 C18 Dy 60.38(15) . . ?
C17 C18 Dy 180.000(1) . . ?
C18 O19 Dy 92.89(15) . . ?
C25 C20 C21 118.9(2) . . ?
C25 C20 C6 123.3(2) . . ?
C21 C20 C6 117.8(2) . . ?
C22 C21 C20 121.0(2) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C21 C22 C23 120.0(2) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 119.2(2) . . ?
C24 C23 C26 121.0(2) . . ?
C22 C23 C26 119.6(2) . . ?
C25 C24 C23 120.4(2) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C20 120.3(2) . . ?
C24 C25 H25 119.9 . . ?
C20 C25 H25 119.9 . . ?
O28 C26 O27 123.3(2) . . ?
O28 C26 C23 117.97(19) . . ?
O27 C26 C23 118.7(2) . . ?
C26 O27 Dy 120.74(14) . 7_557 ?
C26 O28 Dy 167.09(15) . 3_445 ?
C30 C29 C30 117.4(3) . 2_656 ?
C30 C29 C11 121.29(16) . . ?
C30 C29 C11 121.29(16) 2_656 . ?
C31 C30 C29 121.2(2) . . ?
C31 C30 H30 119.4 . . ?
C29 C30 H30 119.4 . . ?
C32 C31 C30 121.1(3) . . ?
C32 C31 H31 119.4 . . ?
C30 C31 H31 119.4 . . ?
C31 C32 C31 117.9(3) 2_656 . ?
C31 C32 C33 121.04(17) 2_656 . ?
C31 C32 C33 121.04(17) . . ?
O34 C33 O34 123.9(4) 2_656 . ?
O34 C33 C32 118.06(18) 2_656 . ?
O34 C33 C32 118.06(18) . . ?
C33 O34 H34 109.8 . . ?
Dy O35 H35A 109.4 . . ?
Dy O35 H35B 51.7 . . ?
H35A O35 H35B 105.3 . . ?
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
Dy O28 2.2546(15) 4_556 ?
Dy O28 2.2547(16) 3 ?
Dy O27 2.3935(16) 7_557 ?
Dy O27 2.3936(16) 8 ?
Dy O35 2.4459(16) 2_656 ?
Dy O35 2.4460(16) . ?
Dy O19 2.4434(16) . ?
Dy O19 2.4434(16) 2_656 ?
Dy C18 2.807(3) . ?
Dy H35B 2.0321 . ?
C1 C2 1.399(3) . ?
C1 C2 1.399(3) 2_656 ?
C1 C14 1.487(5) . ?
C2 N12 1.367(3) . ?
C2 C3 1.446(3) . ?
C3 C4 1.351(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.443(3) . ?
C4 H4 0.9500 . ?
C5 N12 1.370(3) . ?
C5 C6 1.399(3) . ?
C6 C7 1.414(3) . ?
C6 C20 1.500(3) . ?
C7 N13 1.372(3) . ?
C7 C8 1.438(3) . ?
C8 C9 1.358(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.445(3) . ?
C9 H9 0.9500 . ?
C10 N13 1.375(3) . ?
C10 C11 1.413(3) . ?
C11 C10 1.413(3) 2_656 ?
C11 C29 1.482(5) . ?
N12 H12 0.8800 . ?
N13 H13 0.8800 . ?
C14 C15 1.375(3) 2_656 ?
C14 C15 1.375(3) . ?
C15 C16 1.383(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.376(3) . ?
C16 H16 0.9500 . ?
C17 C16 1.376(3) 2_656 ?
C17 C18 1.492(5) . ?
C18 O19 1.264(2) 2_656 ?
C18 O19 1.264(2) . ?
C20 C25 1.390(3) . ?
C20 C21 1.395(3) . ?
C21 C22 1.386(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.394(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.395(3) . ?
C23 C26 1.504(3) . ?
C24 C25 1.395(3) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 O28 1.256(3) . ?
C26 O27 1.265(3) . ?
O27 Dy 2.3936(16) 7_557 ?
O28 Dy 2.2547(15) 3_445 ?
C29 C30 1.399(3) . ?
C29 C30 1.399(3) 2_656 ?
C30 C31 1.393(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.393(3) . ?
C31 H31 0.9500 . ?
C32 C31 1.393(3) 2_656 ?
C32 C33 1.517(5) . ?
C33 O34 1.260(3) 2_656 ?
C33 O34 1.260(3) . ?
O34 H34 0.8117 . ?
O35 H35A 0.9602 . ?
O35 H35B 0.8500 . ?
