#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:11:52 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180172 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/68/7106866.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_7106866
loop_
_publ_author_name
'Gui-Ge Hou'
'Yue Liu'
'Qi-Kui Liu'
'Jian-Ping Ma'
'Yu-Bin Dong'
_publ_section_title
;
 NbO lattice MOFs based on octahedral M(II) and ditopic pyridyl
 substituted diketonate ligands: structure, encapsulation and guest-driven
 luminescent property
;
_journal_coden_Cambridge         182
_journal_name_full               Chem.Commun.
_journal_page_first              10731
_journal_paper_doi               10.1039/c1cc14115e
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C54 H62 Cu3 N6 O19'
_chemical_formula_weight         1289.72
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   26.718(5)
_cell_length_b                   26.718(5)
_cell_length_c                   7.7553(19)
_cell_measurement_reflns_used    2457
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.416
_cell_measurement_theta_min      2.640
_cell_volume                     4794.4(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    0.0347
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8105
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    1.060
_exptl_absorpt_correction_T_max  0.9200
_exptl_absorpt_correction_T_min  0.6194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             2001
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1877
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0460
_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)+(0.0783P)²+1.4160P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1236
_reflns_number_gt                1549
_reflns_number_total             1877
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc14115e.txt
_cod_data_source_block           71023b
_cod_original_cell_volume        4794.3(17)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7106866
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Cu1 Cu 0.3333 0.1667 0.6667 0.0345(2) Uani 1 2 d S
C1 C 0.1815(2) 0.1193(2) 0.3721(6) 0.0905(16) Uani 1 1 d .
H1A H 0.1994 0.1285 0.2605 0.136 Uiso 1 1 calc R
H1B H 0.1554 0.1340 0.3811 0.136 Uiso 1 1 calc R
H1C H 0.1606 0.0782 0.3873 0.136 Uiso 1 1 calc R
C2 C 0.22706(15) 0.14637(16) 0.5086(4) 0.0542(9) Uani 1 1 d .
C3 C 0.22438(16) 0.18590(17) 0.6211(4) 0.0627(10) Uani 1 1 d .
H3 H 0.1975 0.1973 0.5962 0.075 Uiso 1 1 calc R
C4 C 0.25830(13) 0.20955(13) 0.7662(4) 0.0407(7) Uani 1 1 d .
C5 C 0.24182(13) 0.24136(13) 0.8922(4) 0.0393(7) Uani 1 1 d .
C6 C 0.20678(14) 0.26380(14) 0.8509(4) 0.0463(8) Uani 1 1 d .
H6 H 0.1942 0.2622 0.7381 0.056 Uiso 1 1 calc R
C7 C 0.26021(17) 0.24769(17) 1.0617(4) 0.0613(10) Uani 1 1 d .
H7 H 0.2851 0.2346 1.0958 0.074 Uiso 1 1 calc R
C8 C 0.24168(17) 0.27327(18) 1.1797(4) 0.0641(11) Uani 1 1 d .
H8 H 0.2544 0.2766 1.2930 0.077 Uiso 1 1 calc R
C9 C 0.19070(14) 0.28851(15) 0.9778(4) 0.0494(8) Uani 1 1 d .
H9 H 0.1667 0.3030 0.9469 0.059 Uiso 1 1 calc R
N1 N 0.20679(12) 0.29335(12) 1.1414(3) 0.0483(7) Uani 1 1 d .
O1 O 0.30168(9) 0.20490(8) 0.8085(2) 0.0402(5) Uani 1 1 d .
O2 O 0.26452(9) 0.13103(9) 0.5132(3) 0.0460(5) Uani 1 1 d .
O3 O 0.0000 0.0000 0.5000 0.435(17) Uiso 1 6 d SD
O4 O 0.0451(4) 0.0998(7) 0.0845(14) 0.599(14) Uiso 1 1 d D
H4A H 0.0703 0.1359 0.0952 0.719 Uiso 1 1 d RD
H3B H 0.0361 0.0124 0.4833 0.719 Uiso 0.17 1 d PRD
H4B H 0.0367 0.0835 0.1840 0.719 Uiso 1 1 d RD
H3A H -0.0073 0.0128 0.5941 0.719 Uiso 0.17 1 d PRD
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'
Cu Cu 0.3201 1.2651 '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
O1 Cu1 O1 180.0 13_556 .
O1 Cu1 O2 92.81(8) 13_556 13_556
O1 Cu1 O2 87.20(8) . 13_556
O1 Cu1 O2 87.20(8) 13_556 .
O1 Cu1 O2 92.80(8) . .
O2 Cu1 O2 180.0 13_556 .
O1 Cu1 N1 89.94(9) 13_556 11_557
O1 Cu1 N1 90.06(9) . 11_557
O2 Cu1 N1 87.03(9) 13_556 11_557
O2 Cu1 N1 92.97(9) . 11_557
O1 Cu1 N1 90.07(9) 13_556 5_554
O1 Cu1 N1 89.93(9) . 5_554
O2 Cu1 N1 92.97(9) 13_556 5_554
O2 Cu1 N1 87.02(9) . 5_554
N1 Cu1 N1 180.0 11_557 5_554
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
O2 C2 C3 125.3(3) . .
O2 C2 C1 116.7(3) . .
C3 C2 C1 118.0(3) . .
C4 C3 C2 125.6(3) . .
C4 C3 H3 117.2 . .
C2 C3 H3 117.2 . .
O1 C4 C3 126.0(3) . .
O1 C4 C5 115.4(3) . .
C3 C4 C5 118.6(3) . .
C6 C5 C7 116.4(3) . .
C6 C5 C4 123.5(3) . .
C7 C5 C4 120.1(3) . .
C9 C6 C5 119.2(3) . .
C9 C6 H6 120.4 . .
C5 C6 H6 120.4 . .
C8 C7 C5 120.0(3) . .
C8 C7 H7 120.0 . .
C5 C7 H7 120.0 . .
N1 C8 C7 123.7(3) . .
N1 C8 H8 118.1 . .
C7 C8 H8 118.1 . .
N1 C9 C6 124.8(3) . .
N1 C9 H9 117.6 . .
C6 C9 H9 117.6 . .
C8 N1 C9 115.9(3) . .
C8 N1 Cu1 127.6(2) . 9
C9 N1 Cu1 116.5(2) . 9
C4 O1 Cu1 124.06(19) . .
C2 O2 Cu1 123.9(2) . .
H3B O3 H3A 113.9 . .
H4A O4 H4B 109.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.9572(18) 13_556
Cu1 O1 1.9573(18) .
Cu1 O2 1.988(2) 13_556
Cu1 O2 1.988(2) .
Cu1 N1 2.377(2) 11_557
Cu1 N1 2.377(2) 5_554
C1 C2 1.498(5) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 O2 1.258(4) .
C2 C3 1.399(5) .
C3 C4 1.384(4) .
C3 H3 0.9300 .
C4 O1 1.269(3) .
C4 C5 1.498(4) .
C5 C6 1.378(4) .
C5 C7 1.384(5) .
C6 C9 1.368(4) .
C6 H6 0.9300 .
C7 C8 1.374(4) .
C7 H7 0.9300 .
C8 N1 1.321(4) .
C8 H8 0.9300 .
C9 N1 1.325(4) .
C9 H9 0.9300 .
N1 Cu1 2.377(2) 9
O3 H3B 0.8584 .
O3 H3A 0.8681 .
O4 H4A 0.8619 .
O4 H4B 0.8588 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O2 C2 C3 C4 -7.5(6) . .
C1 C2 C3 C4 171.8(4) . .
C2 C3 C4 O1 9.3(6) . .
C2 C3 C4 C5 -167.4(3) . .
O1 C4 C5 C6 162.4(3) . .
C3 C4 C5 C6 -20.5(5) . .
O1 C4 C5 C7 -20.0(5) . .
C3 C4 C5 C7 157.1(4) . .
C7 C5 C6 C9 -2.4(5) . .
C4 C5 C6 C9 175.3(3) . .
C6 C5 C7 C8 2.4(6) . .
C4 C5 C7 C8 -175.4(3) . .
C5 C7 C8 N1 -0.6(7) . .
C5 C6 C9 N1 0.7(5) . .
C7 C8 N1 C9 -1.2(6) . .
C7 C8 N1 Cu1 176.0(3) . 9
C6 C9 N1 C8 1.2(5) . .
C6 C9 N1 Cu1 -176.4(3) . 9
C3 C4 O1 Cu1 4.2(4) . .
C5 C4 O1 Cu1 -178.98(18) . .
O1 Cu1 O1 C4 27(3) 13_556 .
O2 Cu1 O1 C4 167.0(2) 13_556 .
O2 Cu1 O1 C4 -13.0(2) . .
N1 Cu1 O1 C4 -106.0(2) 11_557 .
N1 Cu1 O1 C4 74.0(2) 5_554 .
C3 C2 O2 Cu1 -7.1(5) . .
C1 C2 O2 Cu1 173.6(3) . .
O1 Cu1 O2 C2 -165.5(3) 13_556 .
O1 Cu1 O2 C2 14.4(3) . .
O2 Cu1 O2 C2 -1.8(10) 13_556 .
N1 Cu1 O2 C2 104.7(3) 11_557 .
N1 Cu1 O2 C2 -75.3(3) 5_554 .
