#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/01/2200108.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2200108 loop_ _publ_author_name 'Liang, Yucang' 'Hong, Maochun' 'Cao, Rong' 'Sun, Daofeng' 'Weng, Jiabao' _publ_section_title ; Polymeric tri-\m-oxo(pyrazine)molybdenum(VI) ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m159 _journal_page_last m161 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Mo2 )6 (C4 H4 N2)]' _chemical_formula_moiety 'C4 H4 Mo2 N2 O6' _chemical_formula_sum 'C4 H4 Mo2 N2 O6' _chemical_formula_weight 367.98 _chemical_name_common 'C4 H4 Mo2 N2 O6' _chemical_name_systematic ; ? ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _audit_creation_method SHELXS-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.566(16) _cell_length_b 7.39(2) _cell_length_c 14.04(3) _cell_measurement_reflns_used 2590 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.11 _cell_measurement_theta_min 2.90 _cell_volume 785(3) _computing_cell_refinement 'SMART ' _computing_data_collection 'SMART (Siemens, 1994)' _computing_data_reduction 'SMART ' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device_type 'Siemens Smart CCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0267 _diffrn_reflns_av_sigmaI/netI .0198 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 3627 _diffrn_reflns_theta_max 25.11 _diffrn_reflns_theta_min 2.90 _diffrn_standards_decay_% none _exptl_absorpt_coefficient_mu 3.202 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min .8161 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour black _exptl_crystal_density_diffrn 3.113 _exptl_crystal_density_meas none _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 348 _exptl_crystal_size_max .10 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .06 _refine_diff_density_max 1.093 _refine_diff_density_min -1.114 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.238 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 64 _refine_ls_number_reflns 695 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.238 _refine_ls_R_factor_all .0391 _refine_ls_R_factor_gt .0345 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+18.7425P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0856 _reflns_number_gt 630 _reflns_number_total 695 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bt6019.cif _[local]_cod_data_source_block I _cod_database_code 2200108 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Mo .53153(8) .04406(8) .72799(5) .0094(3) Uani d . 1 . . Mo N1 .5163(10) .0231(9) .9018(5) .0180(15) Uani d . 1 . . N O1 .7602(9) .0276(13) .7470(4) .049(2) Uani d . 1 . . O O2 .5002(13) .2812(8) .7518(5) .049(2) Uani d . 1 . . O O3 .5142(7) .0367(8) .6086(4) .0177(13) Uani d . 1 . . O C1 .6160(12) -.0961(11) .9494(6) .0179(18) Uani d . 1 . . C H1A .6982 -.1651 .9162 .021 Uiso calc R 1 . . H C2 .3998(11) .1193(11) .9540(6) .0159(17) Uani d . 1 . . C H2A .3281 .2038 .9237 .019 Uiso calc R 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mo .0079(4) .0078(4) .0124(4) .0002(3) .0009(3) .0004(3) N1 .025(4) .017(4) .012(3) .000(3) -.002(3) .002(3) O1 .006(3) .121(7) .021(3) .003(4) -.002(3) -.001(4) O2 .117(7) .007(3) .022(3) .003(4) .002(4) .001(3) O3 .017(3) .021(3) .015(3) .000(3) -.001(2) -.001(2) C1 .023(5) .008(4) .022(4) .003(3) .004(4) -.003(3) C2 .014(4) .013(4) .020(4) .004(3) -.001(3) .003(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mo O3 . 1.682(7) yes Mo O1 . 1.755(7) yes Mo O2 . 1.799(8) yes Mo O2 3_646 1.976(9) ? Mo O1 6_557 2.086(8) ? Mo N1 . 2.449(8) yes N1 C1 . 1.338(11) no N1 C2 . 1.349(11) no O1 Mo 6_657 2.086(8) no O2 Mo 3_656 1.976(9) no C1 C2 5_657 1.372(12) no C2 C1 5_657 1.372(12) no loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 .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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 Mo O1 . . 103.1(3) yes O3 Mo O2 . . 101.9(3) yes O1 Mo O2 . . 99.7(5) yes O3 Mo O2 . 3_646 95.9(3) yes O1 Mo O2 . 3_646 91.7(4) yes O2 Mo O2 . 3_646 156.01(9) yes O3 Mo O1 . 6_557 95.1(3) yes O1 Mo O1 . 6_557 160.1(2) yes O2 Mo O1 . 6_557 84.0(4) yes O2 Mo O1 3_646 6_557 78.4(4) yes O3 Mo N1 . . 171.0(3) yes O1 Mo N1 . . 83.7(3) yes O2 Mo N1 . . 82.5(3) yes O2 Mo N1 3_646 . 77.8(3) yes O1 Mo N1 6_557 . 77.4(2) yes C1 N1 C2 . . 116.3(7) no C1 N1 Mo . . 120.9(6) no C2 N1 Mo . . 122.6(5) no Mo O1 Mo . 6_657 172.6(6) no Mo O2 Mo . 3_656 177.5(4) no N1 C1 C2 . 5_657 121.8(8) no N1 C2 C1 . 5_657 121.9(8) no _journal_paper_doi 10.1107/S160053680100441X