#------------------------------------------------------------------------------ #$Date: 2011-03-05 23:30:08 +0200 (Sat, 05 Mar 2011) $ #$Revision: 12742 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/8102003.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_8102003 loop_ _publ_author_name 'Z.-S. Peng' 'W.-J. Jiang' 'Q. Deng' 'Y.-F. Long' 'T.-J. Cai' _publ_section_title ; Refinement of the crystal structure of catena-[(1,10- phenanthroline-N,N')-(µ3-molybdato(VI))copper(II)] monohydrate, Cu(C2H10N2)(MoO4) · H2O ; _journal_issue 3 _journal_name_full 'Zeitschrift f\"ur Kristallographie - New Crystal Structures' _journal_page_first 335 _journal_volume 221 _journal_year 2006 _chemical_formula_moiety 'C12 H8 Cu Mo N2 O4, H2 O' _chemical_formula_structural 'Cu(C~12~H~10~N~2~)(MoO~4~) · H~2~O' _chemical_formula_sum 'C12 H10 Cu Mo N2 O5' _chemical_formula_weight 421.70 _chemical_name_systematic ; catena-[(1,10-phenanthroline)(\m~3~-molybdato(VI))copper(II)] monohydrate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 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 103.271(12) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 14.147(3) _cell_length_b 5.8897(11) _cell_length_c 16.221(3) _cell_measurement_reflns_used 3500 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 2.5 _cell_volume 1315.5(4) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _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_detector_area_resol_mean 0.87 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker SMART APEX CCD II' _diffrn_measurement_method omega _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 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 11008 _diffrn_reflns_theta_full 28.49 _diffrn_reflns_theta_max 28.49 _diffrn_reflns_theta_min 2.58 _diffrn_standards_decay_% negligible _diffrn_standards_interval_count none _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.592 _exptl_absorpt_correction_T_max 0.595 _exptl_absorpt_correction_T_min 0.469 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 2.129 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 828 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.420 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.074 _refine_ls_extinction_coef 0.0008(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 191 _refine_ls_number_reflns 3304 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0228 _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/[\s^2^(Fo^2^)+(0.0285P)^2^+0.8410P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.0606 _reflns_number_gt 2860 _reflns_number_total 3304 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file 1267-1817.cff _[local]_cod_data_source_block '[Cu(MoO4)(C12H10N2)]H2O' _[local]_cod_cif_authors_sg_H-M P12(1)/n1 _[local]_cod_chemical_formula_sum_orig 'C12 H10 Cu1 Mo1 N2 O5' _cod_database_code 8102003 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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_Wyckoff_symbol _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.872034(13) 0.22461(3) 0.015275(12) 0.02307(7) Uani 1 4 e d . . . O1 O 0.85180(11) 0.4868(3) 0.05976(10) 0.0302(3) Uani 1 4 e d . . . O2 O 0.96578(13) 0.2517(3) -0.03918(12) 0.0366(4) Uani 1 4 e d . . . O3 O 0.76572(13) 0.1475(3) -0.05488(12) 0.0446(4) Uani 1 4 e d . . . O4 O 0.90085(12) 0.0179(3) 0.09646(11) 0.0355(4) Uani 1 4 e d . . . Cu1 Cu 0.966540(19) 0.73343(4) 0.127915(17) 0.02390(8) Uani 1 4 e d . . . N1 N 1.04754(13) 0.4678(3) 0.18639(11) 0.0269(4) Uani 1 4 e d . . . N2 N 0.91774(14) 0.7289(3) 0.23466(12) 0.0266(4) Uani 1 4 e d . . . C1 C 1.11103(17) 0.3369(4) 0.16005(15) 0.0323(5) Uani 1 4 e d . . . H1A H 1.1270 0.3714 0.1090 0.039 Uiso 1 4 e calc R . . C2 C 1.15479(18) 0.1492(5) 0.20608(16) 0.0366(6) Uani 1 4 e d . . . H2A H 1.1987 0.0607 0.1854 0.044 Uiso 1 4 e calc R . . C3 C 1.13302(17) 0.0961(4) 0.28126(16) 0.0365(6) Uani 1 4 e d . . . H3A H 1.1627 -0.0270 0.3128 0.044 Uiso 1 4 e calc R . . C4 C 1.06507(17) 0.2296(4) 0.31086(15) 0.0305(5) Uani 1 4 e d . . . C5 C 1.03508(19) 0.1863(5) 0.38774(16) 0.0375(6) Uani 1 4 e d . . . H5A H 1.0621 0.0651 0.4218 0.045 Uiso 1 4 e calc R . . C6 C 0.96786(18) 0.3193(5) 0.41179(15) 0.0364(6) Uani 1 4 e d . . . H6A H 0.9488 0.2858 0.4616 0.044 Uiso 1 4 e calc R . . C7 C 0.92589(16) 0.5093(4) 0.36226(14) 0.0289(5) Uani 1 4 e d . . . C8 C 0.85638(17) 0.6570(5) 0.38307(15) 0.0355(5) Uani 1 4 e d . . . H8A H 0.8351 0.6345 0.4326 0.043 Uiso 1 4 e calc R . . C9 C 0.82049(18) 0.8324(5) 0.33056(16) 0.0365(5) Uani 1 4 e d . . . H9A H 0.7745 0.9299 0.3439 0.044 Uiso 1 4 e calc R . . C10 C 0.85332(17) 0.8649(4) 0.25634(15) 0.0326(5) Uani 1 4 e d . . . H10A H 0.8290 0.9862 0.2212 0.039 Uiso 1 4 e calc R . . C11 C 1.02469(15) 0.4130(4) 0.26085(13) 0.0253(4) Uani 1 4 e d . . . C12 C 0.95405(15) 0.5546(4) 0.28655(13) 0.0247(4) Uani 1 4 e d . . . O1W O 0.68606(16) -0.2763(3) -0.04179(16) 0.0555(6) Uani 1 4 e d . . . H2 H 0.7081 -0.1361 -0.0491 0.075 Uiso 1 4 e d . . . H1 H 0.7330 -0.3562 -0.0073 0.075 Uiso 1 4 e d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.02685(11) 0.02022(11) 0.02524(11) 0.00192(7) 0.01237(8) 0.00067(7) O1 0.0317(8) 0.0243(8) 0.0373(9) -0.0026(7) 0.0132(7) 0.0015(6) O2 0.0461(10) 0.0336(10) 0.0398(10) 0.0077(7) 0.0299(8) 0.0048(7) O3 0.0395(10) 0.0440(11) 0.0462(11) -0.0069(9) 0.0012(8) -0.0051(8) O4 0.0481(10) 0.0296(9) 0.0357(9) 0.0113(7) 0.0238(8) 0.0112(7) Cu1 0.02846(14) 0.02304(15) 0.02372(15) 0.00432(10) 0.01323(11) 0.00354(10) N1 0.0285(9) 0.0294(10) 0.0246(9) 0.0039(8) 0.0097(7) 0.0035(7) N2 0.0286(9) 0.0286(10) 0.0254(9) 0.0027(7) 0.0117(8) 0.0031(7) C1 0.0349(12) 0.0363(13) 0.0286(12) 0.0021(10) 0.0134(10) 0.0064(10) C2 0.0353(12) 0.0368(14) 0.0390(14) -0.0007(11) 0.0111(11) 0.0114(11) C3 0.0369(13) 0.0345(14) 0.0368(13) 0.0064(11) 0.0057(10) 0.0099(10) C4 0.0299(11) 0.0329(13) 0.0277(12) 0.0043(9) 0.0042(9) 0.0027(9) C5 0.0421(14) 0.0412(14) 0.0288(12) 0.0138(11) 0.0070(11) 0.0068(11) C6 0.0422(13) 0.0453(15) 0.0242(11) 0.0095(11) 0.0127(10) 0.0008(11) C7 0.0285(11) 0.0354(13) 0.0241(11) 0.0019(9) 0.0090(9) -0.0021(9) C8 0.0361(12) 0.0468(15) 0.0283(12) 0.0002(11) 0.0171(10) -0.0013(11) C9 0.0339(12) 0.0424(15) 0.0377(13) -0.0015(12) 0.0178(10) 0.0066(11) C10 0.0348(12) 0.0319(13) 0.0337(12) 0.0028(10) 0.0134(10) 0.0084(10) C11 0.0252(10) 0.0281(11) 0.0225(10) 0.0015(9) 0.0057(8) 0.0001(8) C12 0.0259(10) 0.0264(11) 0.0223(10) 0.0016(8) 0.0067(8) -0.0011(8) O1W 0.0434(11) 0.0414(12) 0.0775(17) -0.0070(10) 0.0049(11) -0.0051(9) 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' Mo Mo -1.6832 0.6857 '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 O3 Mo1 O1 107.63(8) . . ? O3 Mo1 O2 109.62(9) . . ? O1 Mo1 O2 109.81(7) . . ? O3 Mo1 O4 109.05(9) . . ? O1 Mo1 O4 109.30(8) . . ? O2 Mo1 O4 111.35(8) . . ? Mo1 O1 Cu1 126.71(8) . . ? Mo1 O2 Cu1 161.80(13) . 3_765 ? Mo1 O4 Cu1 144.03(9) . 1_545 ? O2 Cu1 O4 93.18(7) 3_765 1_565 ? O2 Cu1 N2 170.08(8) 3_765 . ? O4 Cu1 N2 89.98(7) 1_565 . ? O2 Cu1 N1 93.47(7) 3_765 . ? O4 Cu1 N1 167.21(8) 1_565 . ? N2 Cu1 N1 81.73(7) . . ? O2 Cu1 O1 95.09(7) 3_765 . ? O4 Cu1 O1 100.37(7) 1_565 . ? N2 Cu1 O1 93.59(7) . . ? N1 Cu1 O1 89.91(7) . . ? C1 N1 C11 117.69(19) . . ? C1 N1 Cu1 130.21(16) . . ? C11 N1 Cu1 111.89(14) . . ? C10 N2 C12 118.8(2) . . ? C10 N2 Cu1 128.11(16) . . ? C12 N2 Cu1 113.01(14) . . ? N1 C1 C2 122.5(2) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 119.8(2) . . ? C3 C2 H2A 120.1 . . ? C1 C2 H2A 120.1 . . ? C2 C3 C4 119.3(2) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C11 C4 C3 117.1(2) . . ? C11 C4 C5 118.8(2) . . ? C3 C4 C5 124.1(2) . . ? C6 C5 C4 121.1(2) . . ? C6 C5 H5A 119.5 . . ? C4 C5 H5A 119.5 . . ? C5 C6 C7 121.3(2) . . ? C5 C6 H6A 119.3 . . ? C7 C6 H6A 119.3 . . ? C12 C7 C8 116.5(2) . . ? C12 C7 C6 118.6(2) . . ? C8 C7 C6 124.9(2) . . ? C9 C8 C7 119.9(2) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 119.5(2) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? N2 C10 C9 122.1(2) . . ? N2 C10 H10A 118.9 . . ? C9 C10 H10A 118.9 . . ? N1 C11 C4 123.6(2) . . ? N1 C11 C12 116.33(19) . . ? C4 C11 C12 120.1(2) . . ? N2 C12 C7 123.2(2) . . ? N2 C12 C11 116.79(19) . . ? C7 C12 C11 120.1(2) . . ? H2 O1W H1 109.5 . . ? 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 Mo1 O3 1.7256(18) . ? Mo1 O1 1.7557(16) . ? Mo1 O2 1.7615(16) . ? Mo1 O4 1.7711(16) . ? O1 Cu1 2.2677(16) . ? O2 Cu1 1.9049(16) 3_765 ? O4 Cu1 1.9269(16) 1_545 ? Cu1 O2 1.9049(16) 3_765 ? Cu1 O4 1.9269(16) 1_565 ? Cu1 N2 2.0061(19) . ? Cu1 N1 2.0398(19) . ? N1 C1 1.327(3) . ? N1 C11 1.359(3) . ? N2 C10 1.320(3) . ? N2 C12 1.352(3) . ? C1 C2 1.397(4) . ? C1 H1A 0.9300 . ? C2 C3 1.361(3) . ? C2 H2A 0.9300 . ? C3 C4 1.409(3) . ? C3 H3A 0.9300 . ? C4 C11 1.392(3) . ? C4 C5 1.429(3) . ? C5 C6 1.356(4) . ? C5 H5A 0.9300 . ? C6 C7 1.425(3) . ? C6 H6A 0.9300 . ? C7 C12 1.401(3) . ? C7 C8 1.411(3) . ? C8 C9 1.361(4) . ? C8 H8A 0.9300 . ? C9 C10 1.400(3) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.435(3) . ? O1W H2 0.9006 . ? O1W H1 0.8968 . ?