#------------------------------------------------------------------------------ #$Date: 2025-08-18 23:52:38 +0100 (Mon, 18 Aug 2025) $ #$Revision: 301791 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/49/2004908.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_2004908 loop_ _publ_author_name 'Fun, H.-K.' 'Sivakumar, K.' 'Niu, J.-Y.' 'Wang, J.-P.' 'You, X.-Z.' _publ_section_title cis-Bis(2-methyl-8-quinolinolato-N,O)dioxomolybdenum(VI) _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1150 _journal_page_last 1152 _journal_paper_doi 10.1107/S0108270195016933 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '[Mo (C10 H8 N1 O1)2 (O)2]' _chemical_formula_sum 'C20 H16 Mo N2 O4' _chemical_formula_weight 444.29 _chemical_name_systematic ; Bis(2-methyl-8-quinolinolato) Molybdenum ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _audit_creation_method SHELXL _cell_angle_alpha 90 _cell_angle_beta 109.4590(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.3698(2) _cell_length_b 8.58030(10) _cell_length_c 16.55730(10) _cell_measurement_reflns_used 6199 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 26.30 _cell_measurement_theta_min 1.62 _cell_volume 1790.91(4) _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_collection 'ASTRO (Siemens, 1995)' _computing_data_reduction SAINT _computing_molecular_graphics SHELXTL/PC _computing_publication_material 'SHELXL93. Geometrical calculations: PARST (Nardelli, 1983)' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXTL/PC (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Siemens SMART area-detector' _diffrn_measurement_method \w _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 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 6199 _diffrn_reflns_theta_max 26.30 _diffrn_reflns_theta_min 1.62 _exptl_absorpt_coefficient_mu 0.761 _exptl_absorpt_correction_type none _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 896 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.31 _refine_diff_density_min -0.33 _refine_ls_extinction_coef 0.0036(3) _refine_ls_extinction_method SHELXL93 _refine_ls_goodness_of_fit_all 1.143 _refine_ls_goodness_of_fit_obs 1.144 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 309 _refine_ls_number_reflns 3301 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.143 _refine_ls_restrained_S_obs 1.144 _refine_ls_R_factor_all 0.0238 _refine_ls_R_factor_obs 0.0229 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0066P)^2^ + 2.1247P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_wR_factor_all 0.0556 _refine_ls_wR_factor_obs 0.0552 _reflns_number_observed 3246 _reflns_number_total 3301 _reflns_observed_criterion I>2sigma(I) _cod_data_source_file mu1231.cif _cod_data_source_block niu31m _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2004908 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 0.01752(11) 0.01990(11) 0.01654(11) -0.00030(7) 0.00316(7) 0.00146(6) N1 0.0160(8) 0.0222(9) 0.0173(8) 0.0002(7) 0.0054(6) 0.0005(7) N2 0.0203(9) 0.0212(9) 0.0182(8) 0.0037(7) 0.0046(7) -0.0003(7) O1 0.0211(7) 0.0222(7) 0.0230(7) -0.0015(6) 0.0010(6) -0.0009(6) O2 0.0201(7) 0.0305(8) 0.0165(7) -0.0019(6) 0.0043(6) -0.0025(6) O3 0.0294(8) 0.0235(8) 0.0268(8) 0.0013(7) 0.0020(6) 0.0029(6) O4 0.0265(8) 0.0319(8) 0.0256(8) -0.0002(7) 0.0104(6) 0.0022(7) C1 0.0169(10) 0.0282(11) 0.0192(10) 0.0030(9) 0.0048(8) -0.0017(8) C2 0.0218(11) 0.0336(13) 0.0241(11) 0.0012(10) 0.0040(9) -0.0065(9) C3 0.0223(11) 0.0488(15) 0.0184(11) 0.0048(11) -0.0004(9) -0.0047(10) C4 0.0244(11) 0.0426(14) 0.0209(11) 0.0074(10) 0.0052(9) 0.0059(10) C5 0.0192(10) 0.0327(12) 0.0200(10) 0.0045(9) 0.0093(8) 0.0054(9) C6 0.0246(11) 0.0276(11) 0.0284(11) 0.0058(9) 0.0130(9) 0.0085(9) C7 0.0255(11) 0.0200(11) 0.0309(12) 0.0002(9) 0.0146(9) 0.0021(9) C8 0.0176(10) 0.0240(10) 0.0218(10) -0.0007(8) 0.0097(8) 0.0006(8) C9 0.0158(10) 0.0280(11) 0.0178(10) 0.0025(8) 0.0070(8) 0.0006(8) C10 0.0261(12) 0.0231(11) 0.0260(11) -0.0021(9) 0.0068(9) -0.0037(9) C11 0.0184(10) 0.0254(11) 0.0220(10) 0.0023(9) 0.0058(8) -0.0003(8) C12 0.0212(11) 0.0341(12) 0.0266(11) -0.0009(10) 0.0039(9) -0.0067(10) C13 0.0204(11) 0.0363(13) 0.0410(14) -0.0041(10) 0.0062(10) -0.0089(11) C14 0.0225(12) 0.0359(13) 0.0453(14) -0.0027(10) 0.0176(11) -0.0036(11) C15 0.0230(11) 0.0265(11) 0.0304(12) 0.0034(9) 0.0115(9) -0.0002(9) C16 0.0351(14) 0.0367(13) 0.0350(13) 0.0013(11) 0.0216(11) -0.0017(11) C17 0.0388(14) 0.0385(13) 0.0230(11) 0.0056(11) 0.0143(10) -0.0048(10) C18 0.0263(11) 0.0258(11) 0.0197(10) 0.0061(9) 0.0049(8) -0.0010(8) C19 0.0194(10) 0.0211(10) 0.0215(10) 0.0029(8) 0.0050(8) -0.0005(8) C20 0.0315(13) 0.045(2) 0.0265(12) 0.0005(12) 0.0061(11) -0.0158(11) loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_type_symbol Mo 1 .746823(13) .15256(2) .106914(10) .01862(8) Uani d Mo N1 1 .68030(13) .3970(2) .03812(10) .0185(3) Uani d N N2 1 .85932(14) .1726(2) .01384(11) .0204(4) Uani d N O1 1 .62936(11) .0997(2) .00005(9) .0237(3) Uani d O O2 1 .87571(11) .2691(2) .17166(9) .0228(3) Uani d O O3 1 .78954(13) -.0384(2) .12405(10) .0284(4) Uani d O O4 1 .68206(12) .1876(2) .17916(10) .0276(3) Uani d O C1 1 .5771(2) .2072(3) -.05969(13) .0217(4) Uani d C C2 1 .4984(2) .1664(3) -0.13632(14) .0274(5) Uani d C C3 1 .4472(2) .2864(3) -0.19557(14) .0316(5) Uani d C C4 1 .4707(2) .4421(3) -0.17812(14) .0299(5) Uani d C C5 1 .5494(2) .4872(3) -.09871(13) .0233(4) Uani d C C6 1 .5746(2) .6437(3) -.07057(15) .0258(5) Uani d C C7 1 .6469(2) .6727(3) .00931(15) .0242(4) Uani d C C8 1 .6996(2) .5466(2) .06402(13) .0203(4) Uani d C C9 1 .6038(2) .3676(2) -.04086(13) .0202(4) Uani d C C10 1 .7764(2) .5817(3) .15304(14) .0255(5) Uani d C C11 1 .9569(2) .3074(3) .14243(13) .0222(4) Uani d C C12 1 1.0443(2) .3932(3) .19175(15) .0283(5) Uani d C C13 1 1.1273(2) .4286(3) .1587(2) .0336(5) Uani d C C14 1 1.1232(2) .3780(3) .0786(2) .0330(5) Uani d C C15 1 1.0344(2) .2887(3) .02683(14) .0260(5) Uani d C C16 1 1.0244(2) .2245(3) -.0552(2) .0331(5) Uani d C C17 1 .9361(2) .1383(3) -.09833(15) .0325(5) Uani d C C18 1 .8534(2) .1125(3) -.06299(13) .0246(5) Uani d C C19 1 .9498(2) .2563(2) .05844(13) .0211(4) Uani d C C20 1 .7595(2) .0141(3) -0.1129(2) .0351(6) Uani d C H2 1 .4810(19) .061(3) -0.1465(15) .024(6) Uiso d H H3 1 .396(2) .253(3) -0.2478(17) .035(7) Uiso d H H4 1 .436(2) .527(3) -0.2179(16) .032(7) Uiso d H H6 1 .538(2) .723(3) -0.1053(16) .029(7) Uiso d H H7 1 .6625(18) .774(3) .0273(15) .021(6) Uiso d H H10A 1 .7684(19) .508(3) .1929(15) .024(6) Uiso d H H10B 1 .848(2) .575(3) .1530(17) .036(7) Uiso d H H10C 1 .764(2) .687(3) .1707(16) .032(7) Uiso d H H12 1 1.047(2) .430(3) .2482(18) .042(8) Uiso d H H13 1 1.185(2) .490(3) .1930(16) .030(7) Uiso d H H14 1 1.181(2) .402(4) .0572(18) .047(8) Uiso d H H16 1 1.078(2) .236(4) -.0735(18) .043(8) Uiso d H H17 1 .927(2) .095(3) -0.1530(18) .038(7) Uiso d H H20A 1 .780(2) -.061(3) -0.1481(17) .036(7) Uiso d H H20B 1 .700(3) .074(4) -0.148(2) .050(9) Uiso d H H20C 1 .727(3) -.043(4) -.075(2) .051(9) Uiso d H 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' 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_publ_flag O4 Mo O3 105.49(8) yes O4 Mo O2 94.84(7) yes O3 Mo O2 102.15(7) yes O4 Mo O1 103.14(7) yes O3 Mo O1 92.86(7) yes O2 Mo O1 152.61(6) yes O4 Mo N1 89.11(7) yes O3 Mo N1 162.29(7) yes O2 Mo N1 86.20(6) yes O1 Mo N1 73.74(6) yes O4 Mo N2 164.77(7) yes O3 Mo N2 86.12(7) yes O2 Mo N2 72.73(6) yes O1 Mo N2 85.75(6) yes N1 Mo N2 81.46(6) yes C8 N1 C9 118.3(2) ? C8 N1 Mo 132.48(13) ? C9 N1 Mo 109.09(13) ? C18 N2 C19 117.7(2) ? C18 N2 Mo 134.29(15) ? C19 N2 Mo 107.76(12) ? C1 O1 Mo 123.66(13) ? C11 O2 Mo 125.62(12) ? O1 C1 C2 122.6(2) ? O1 C1 C9 117.5(2) ? C2 C1 C9 119.8(2) ? C1 C2 C3 119.1(2) ? C4 C3 C2 122.0(2) ? C3 C4 C5 119.9(2) ? C6 C5 C9 116.5(2) ? C6 C5 C4 125.1(2) ? C9 C5 C4 118.3(2) ? C7 C6 C5 119.9(2) ? C6 C7 C8 120.6(2) ? N1 C8 C7 121.0(2) ? N1 C8 C10 119.5(2) ? C7 C8 C10 119.5(2) ? N1 C9 C5 123.5(2) ? N1 C9 C1 115.6(2) ? C5 C9 C1 120.8(2) ? O2 C11 C12 122.0(2) ? O2 C11 C19 117.8(2) ? C12 C11 C19 120.2(2) ? C11 C12 C13 119.8(2) ? C14 C13 C12 121.0(2) ? C13 C14 C15 120.2(2) ? C19 C15 C16 116.1(2) ? C19 C15 C14 119.1(2) ? C16 C15 C14 124.8(2) ? C17 C16 C15 119.5(2) ? C16 C17 C18 121.2(2) ? N2 C18 C17 121.0(2) ? N2 C18 C20 120.4(2) ? C17 C18 C20 118.6(2) ? N2 C19 C15 124.3(2) ? N2 C19 C11 116.0(2) ? C15 C19 C11 119.6(2) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Mo O4 1.721(2) yes Mo O3 1.727(2) yes Mo O2 1.9717(14) yes Mo O1 1.9878(14) yes Mo N1 2.411(2) yes Mo N2 2.492(2) yes N1 C8 1.350(3) ? N1 C9 1.389(3) ? N2 C18 1.350(3) ? N2 C19 1.389(3) ? O1 C1 1.362(3) ? O2 C11 1.368(3) ? C1 C2 1.396(3) ? C1 C9 1.430(3) ? C2 C3 1.429(3) ? C3 C4 1.381(4) ? C4 C5 1.437(3) ? C5 C6 1.424(3) ? C5 C9 1.427(3) ? C6 C7 1.376(3) ? C7 C8 1.436(3) ? C8 C10 1.520(3) ? C11 C12 1.392(3) ? C11 C19 1.431(3) ? C12 C13 1.424(4) ? C13 C14 1.378(4) ? C14 C15 1.433(3) ? C15 C19 1.422(3) ? C15 C16 1.430(3) ? C16 C17 1.374(4) ? C17 C18 1.430(3) ? C18 C20 1.510(3) ? loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139054921