#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:41:49 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179731 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/27/7002737.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_7002737
loop_
_publ_author_name
'Rodríguez-Diéguez, Antonio'
'Mota, Antonio J.'
'Seco, José M.'
'Palacios, María A.'
'Romerosa, Antonio'
'Colacio, Enrique'
_publ_section_title
;
 Influence of metal ions, coligands and reaction conditions on the
 structural versatility and properties of 5-pyrimidyl-tetrazolate
 containing complexes
;
_journal_issue                   43
_journal_name_full               'Dalton Transactions'
_journal_page_first              9578
_journal_page_last               9586
_journal_paper_doi               10.1039/b910811d
_journal_year                    2009
_chemical_formula_sum            'C30 H18 Dy2 N36 O12'
_chemical_formula_weight         1399.80
_chemical_name_systematic
;
?
;
_space_group_IT_number           54
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2ac'
_symmetry_space_group_name_H-M   'P c c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.844(3)
_cell_length_b                   11.4283(14)
_cell_length_c                   19.349(3)
_cell_measurement_reflns_used    9087
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.615
_cell_measurement_theta_min      2.248
_cell_volume                     5051.4(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker Axs APEX automatic diffractometer'
_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  0.0565
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11047
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    3.029
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5650
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.578
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         4225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0391
_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)+(0.0465P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                2943
_reflns_number_total             4225
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b910811d.txt
_cod_data_source_block           compound8
_cod_original_sg_symbol_H-M      Pcca
_cod_database_code               7002737
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'x+1/2, -y, -z+1/2'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'-x-1/2, y, z-1/2'
'x, -y, 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
Dy3 Dy 0.352322(12) 0.20295(3) 0.464160(15) 0.02740(12) Uani 1 1 d . . .
O2 O 0.38398(18) 0.3948(4) 0.4937(2) 0.0370(11) Uani 1 1 d . . .
O3 O 0.40283(18) 0.1561(4) 0.5685(2) 0.0400(12) Uani 1 1 d . . .
N7B N 0.4659(2) 0.2056(5) 0.4332(3) 0.0346(14) Uani 1 1 d . . .
N7A N 0.2855(2) 0.2956(5) 0.5706(3) 0.0355(14) Uani 1 1 d . . .
N7F N 0.2875(2) 0.0738(5) 0.3756(2) 0.0310(13) Uani 1 1 d . . .
N11B N 0.5506(2) 0.0858(5) 0.4130(3) 0.0395(15) Uani 1 1 d . . .
N11A N 0.1960(2) 0.3940(5) 0.5951(3) 0.0448(16) Uani 1 1 d . . .
N1B N 0.3972(2) 0.0113(5) 0.4357(3) 0.0381(14) Uani 1 1 d . . .
N1A N 0.2619(2) 0.3078(5) 0.4328(3) 0.0339(13) Uani 1 1 d . . .
N1F N 0.2864(2) 0.0621(5) 0.5198(2) 0.0335(13) Uani 1 1 d . . .
N2B N 0.3764(3) -0.0991(6) 0.4328(3) 0.0475(16) Uani 1 1 d . . .
N2A N 0.2396(3) 0.3353(5) 0.3699(3) 0.0470(16) Uani 1 1 d . . .
N2F N 0.2717(3) 0.0373(5) 0.5854(3) 0.0526(18) Uani 1 1 d . . .
N3B N 0.4194(3) -0.1712(5) 0.4219(3) 0.0487(17) Uani 1 1 d . . .
N3A N 0.1931(3) 0.4004(5) 0.3784(3) 0.0517(17) Uani 1 1 d . . .
N4B N 0.4712(3) -0.1107(5) 0.4183(3) 0.0433(15) Uani 1 1 d . . .
N4A N 0.1830(2) 0.4169(5) 0.4460(3) 0.0447(16) Uani 1 1 d . . .
C8B C 0.5003(3) 0.3002(7) 0.4291(4) 0.0445(18) Uani 1 1 d . . .
H2B H 0.4835 0.3738 0.4341 0.053 Uiso 1 1 calc R . .
C8A C 0.2946(3) 0.2849(6) 0.6381(4) 0.0460(19) Uani 1 1 d . . .
H2D H 0.3284 0.2473 0.6530 0.055 Uiso 1 1 calc R . .
C8F C 0.2876(3) 0.0707(7) 0.3064(3) 0.046(2) Uani 1 1 d . . .
C9B C 0.5607(3) 0.2923(8) 0.4173(4) 0.054(2) Uani 1 1 d . . .
H3B H 0.5844 0.3584 0.4147 0.065 Uiso 1 1 calc R . .
C9A C 0.2563(4) 0.3270(6) 0.6869(4) 0.051(2) Uani 1 1 d . . .
H3D H 0.2634 0.3195 0.7341 0.061 Uiso 1 1 calc R . .
C9F C 0.2500 0.0000 0.2687(5) 0.058(3) Uani 1 2 d S . .
C10B C 0.5828(3) 0.1813(8) 0.4099(4) 0.053(2) Uani 1 1 d . . .
H4B H 0.6228 0.1730 0.4023 0.063 Uiso 1 1 calc R . .
C10A C 0.2068(3) 0.3806(7) 0.6618(4) 0.057(2) Uani 1 1 d . . .
H4D H 0.1796 0.4091 0.6933 0.068 Uiso 1 1 calc R . .
C6B C 0.4934(3) 0.1029(6) 0.4243(3) 0.0341(17) Uani 1 1 d . . .
C6A C 0.2356(3) 0.3508(6) 0.5528(3) 0.0323(16) Uani 1 1 d . . .
C6F C 0.2500 0.0000 0.4064(4) 0.027(2) Uani 1 2 d S . .
C5B C 0.4555(3) 0.0020(6) 0.4273(3) 0.0336(17) Uani 1 1 d . . .
C5A C 0.2256(3) 0.3602(6) 0.4790(3) 0.0333(16) Uani 1 1 d . . .
C5F C 0.2500 0.0000 0.4813(4) 0.027(2) Uani 1 2 d S . .
N2R N 0.4727(3) 0.3978(7) 0.2617(4) 0.079(2) Uani 1 1 d . . .
N7R N 0.4466(5) 0.0448(8) 0.2574(4) 0.111(4) Uani 1 1 d . . .
N1R N 0.4543(3) 0.2873(7) 0.2696(4) 0.070(2) Uani 1 1 d . . .
C7R C 0.4486(6) -0.0759(12) 0.2554(6) 0.135(5) Uiso 1 1 d . . .
H2R H 0.4145 -0.1200 0.2578 0.162 Uiso 1 1 calc R . .
C8R C 0.5000 -0.1272(16) 0.2500 0.112(5) Uiso 1 2 d S . .
H3R H 0.5000 -0.2086 0.2500 0.134 Uiso 1 2 calc SR . .
C6R C 0.5000 0.0914(15) 0.2500 0.080(5) Uani 1 2 d S . .
C5R C 0.5000 0.2239(12) 0.2500 0.060(3) Uani 1 2 d S . .
O1W O 0.0694(2) 0.3909(6) 0.1235(3) 0.0823(19) Uani 1 1 d . . .
O2W O 0.0467(2) 0.4026(5) 0.3994(4) 0.086(2) Uani 1 1 d . . .
O3W O 0.1133(3) 0.4299(7) 0.2560(3) 0.114(3) Uani 1 1 d . . .
O1 O 0.36357(19) 0.2857(4) 0.3532(2) 0.0452(13) Uani 1 1 d . . .
H3F H 0.2500 0.0000 0.214(5) 0.05(3) Uiso 1 2 d S . .
H2F H 0.314(3) 0.126(6) 0.279(4) 0.07(2) 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'
Dy Dy -0.1892 4.4098 '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'
H H 0.0000 0.0000 '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
O1 Dy3 O2 79.40(16) . . ?
O1 Dy3 O3 143.79(14) . . ?
O2 Dy3 O3 81.76(16) . . ?
O1 Dy3 N1F 136.79(16) . . ?
O2 Dy3 N1F 133.33(15) . . ?
O3 Dy3 N1F 77.21(16) . . ?
O1 Dy3 N1A 70.88(16) . . ?
O2 Dy3 N1A 82.30(16) . . ?
O3 Dy3 N1A 136.30(17) . . ?
N1F Dy3 N1A 84.95(18) . . ?
O1 Dy3 N1B 96.16(17) . . ?
O2 Dy3 N1B 137.86(17) . . ?
O3 Dy3 N1B 77.83(17) . . ?
N1F Dy3 N1B 76.81(18) . . ?
N1A Dy3 N1B 136.18(18) . . ?
O1 Dy3 N7B 71.63(16) . . ?
O2 Dy3 N7B 75.37(16) . . ?
O3 Dy3 N7B 73.83(15) . . ?
N1F Dy3 N7B 134.78(18) . . ?
N1A Dy3 N7B 139.12(17) . . ?
N1B Dy3 N7B 63.71(18) . . ?
O1 Dy3 N7F 72.67(15) . . ?
O2 Dy3 N7F 145.32(15) . . ?
O3 Dy3 N7F 132.72(16) . . ?
N1F Dy3 N7F 65.37(15) . . ?
N1A Dy3 N7F 69.52(16) . . ?
N1B Dy3 N7F 66.66(16) . . ?
N7B Dy3 N7F 113.41(16) . . ?
O1 Dy3 N7A 125.63(16) . . ?
O2 Dy3 N7A 68.72(15) . . ?
O3 Dy3 N7A 73.97(16) . . ?
N1F Dy3 N7A 65.59(16) . . ?
N1A Dy3 N7A 62.34(17) . . ?
N1B Dy3 N7A 136.82(17) . . ?
N7B Dy3 N7A 134.35(17) . . ?
N7F Dy3 N7A 112.18(16) . . ?
C8B N7B C6B 115.0(6) . . ?
C8B N7B Dy3 126.5(4) . . ?
C6B N7B Dy3 118.4(4) . . ?
C8A N7A C6A 115.3(6) . . ?
C8A N7A Dy3 127.5(5) . . ?
C6A N7A Dy3 117.0(4) . . ?
C8F N7F C6F 115.3(6) . . ?
C8F N7F Dy3 130.3(5) . . ?
C6F N7F Dy3 114.4(4) . . ?
C10B N11B C6B 115.6(6) . . ?
C6A N11A C10A 115.8(7) . . ?
C5B N1B N2B 105.6(6) . . ?
C5B N1B Dy3 120.4(5) . . ?
N2B N1B Dy3 133.6(4) . . ?
N2A N1A C5A 105.0(5) . . ?
N2A N1A Dy3 130.4(4) . . ?
C5A N1A Dy3 124.4(4) . . ?
C5F N1F N2F 105.2(5) . . ?
C5F N1F Dy3 119.4(4) . . ?
N2F N1F Dy3 134.9(4) . . ?
N3B N2B N1B 109.5(6) . . ?
N3A N2A N1A 108.9(6) . . ?
N2F N2F N1F 109.0(3) 2 . ?
N2B N3B N4B 109.9(6) . . ?
N2A N3A N4A 109.9(6) . . ?
C5B N4B N3B 104.1(6) . . ?
C5A N4A N3A 105.9(6) . . ?
N7B C8B C9B 122.4(7) . . ?
N7B C8B H2B 118.8 . . ?
C9B C8B H2B 118.8 . . ?
N7A C8A C9A 123.0(7) . . ?
N7A C8A H2D 118.5 . . ?
C9A C8A H2D 118.5 . . ?
N7F C8F C9F 122.7(8) . . ?
N7F C8F H2F 120(4) . . ?
C9F C8F H2F 117(4) . . ?
C10B C9B C8B 116.0(7) . . ?
C10B C9B H3B 122.0 . . ?
C8B C9B H3B 122.0 . . ?
C10A C9A C8A 115.9(7) . . ?
C10A C9A H3D 122.1 . . ?
C8A C9A H3D 122.1 . . ?
C8F C9F C8F 116.5(10) . 2 ?
C8F C9F H3F 121.8(5) . . ?
C8F C9F H3F 121.8(5) 2 . ?
N11B C10B C9B 123.7(7) . . ?
N11B C10B H4B 118.1 . . ?
C9B C10B H4B 118.1 . . ?
N11A C10A C9A 123.4(7) . . ?
N11A C10A H4D 118.3 . . ?
C9A C10A H4D 118.3 . . ?
N11B C6B N7B 127.3(7) . . ?
N11B C6B C5B 118.4(6) . . ?
N7B C6B C5B 114.3(6) . . ?
N11A C6A N7A 126.6(6) . . ?
N11A C6A C5A 118.5(6) . . ?
N7A C6A C5A 114.9(6) . . ?
N7F C6F N7F 127.4(8) 2 . ?
N7F C6F C5F 116.3(4) 2 . ?
N7F C6F C5F 116.3(4) . . ?
N1B C5B N4B 110.8(6) . . ?
N1B C5B C6B 122.4(6) . . ?
N4B C5B C6B 126.7(6) . . ?
N4A C5A N1A 110.2(6) . . ?
N4A C5A C6A 128.5(6) . . ?
N1A C5A C6A 121.3(6) . . ?
N1F C5F N1F 111.5(7) . 2 ?
N1F C5F C6F 124.3(4) . . ?
N1F C5F C6F 124.3(4) 2 . ?
N2R N2R N1R 109.4(4) 4_655 . ?
C6R N7R C7R 111.3(14) . . ?
C5R N1R N2R 103.7(8) . . ?
C8R C7R N7R 118.5(16) . . ?
C8R C7R H2R 120.7 . . ?
N7R C7R H2R 120.7 . . ?
C7R C8R C7R 127(2) 4_655 . ?
C7R C8R H3R 116.4 4_655 . ?
C7R C8R H3R 116.4 . . ?
N7R C6R N7R 133.1(17) 4_655 . ?
N7R C6R C5R 113.4(8) 4_655 . ?
N7R C6R C5R 113.4(8) . . ?
N1R C5R N1R 113.7(12) 4_655 . ?
N1R C5R C6R 123.2(6) 4_655 . ?
N1R C5R C6R 123.2(6) . . ?
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
Dy3 O1 2.360(4) . ?
Dy3 O2 2.379(5) . ?
Dy3 O3 2.385(4) . ?
Dy3 N1F 2.454(5) . ?
Dy3 N1A 2.464(5) . ?
Dy3 N1B 2.480(6) . ?
Dy3 N7B 2.662(5) . ?
Dy3 N7F 2.703(5) . ?
Dy3 N7A 2.775(5) . ?
N7B C8B 1.339(8) . ?
N7B C6B 1.342(7) . ?
N7A C8A 1.328(8) . ?
N7A C6A 1.348(8) . ?
N7F C8F 1.340(8) . ?
N7F C6F 1.341(6) . ?
N11B C10B 1.317(9) . ?
N11B C6B 1.339(8) . ?
N11A C6A 1.317(8) . ?
N11A C10A 1.323(9) . ?
N1B C5B 1.345(8) . ?
N1B N2B 1.349(8) . ?
N1A N2A 1.355(7) . ?
N1A C5A 1.358(8) . ?
N1F C5F 1.322(6) . ?
N1F N2F 1.344(7) . ?
N2B N3B 1.299(8) . ?
N2A N3A 1.308(7) . ?
N2F N2F 1.308(11) 2 ?
N3B N4B 1.372(8) . ?
N3A N4A 1.342(8) . ?
N4B C5B 1.349(8) . ?
N4A C5A 1.331(8) . ?
C8B C9B 1.403(10) . ?
C8B H2B 0.9300 . ?
C8A C9A 1.374(10) . ?
C8A H2D 0.9300 . ?
C8F C9F 1.388(9) . ?
C8F H2F 1.02(7) . ?
C9B C10B 1.373(10) . ?
C9B H3B 0.9300 . ?
C9A C10A 1.374(10) . ?
C9A H3D 0.9300 . ?
C9F C8F 1.388(9) 2 ?
C9F H3F 1.05(9) . ?
C10B H4B 0.9300 . ?
C10A H4D 0.9300 . ?
C6B C5B 1.443(9) . ?
C6A C5A 1.450(9) . ?
C6F N7F 1.341(6) 2 ?
C6F C5F 1.450(11) . ?
C5F N1F 1.322(6) 2 ?
N2R N2R 1.328(12) 4_655 ?
N2R N1R 1.338(8) . ?
N7R C6R 1.339(10) . ?
N7R C7R 1.380(13) . ?
N1R C5R 1.325(9) . ?
C7R C8R 1.316(13) . ?
C7R H2R 0.9300 . ?
C8R C7R 1.316(13) 4_655 ?
C8R H3R 0.9300 . ?
C6R N7R 1.339(10) 4_655 ?
C6R C5R 1.515(18) . ?
C5R N1R 1.325(9) 4_655 ?
