# Copyright The Royal Society of Chemistry, 1998 # 8/03295E/DAP data_global #======================================================================= # TITLE AND AUTHOR LIST _publ_section_title ; Vibrational and Crystallographic Studies of Dioxohalogenomolybdenum(VI) complexes of Crown Ethers. ; loop_ _publ_author_name _publ_author_address 'Taylor, Michael J.' ; Department of Chemistry University of Auckland Private Bag 92019 Auckland New Zealand ; 'Rickard, Clifton E. F.' ; Department of Chemistry University of Auckland Private Bag 92019 Auckland New Zealand ; 'Kloo, Lars A.' ; Inorganic Chemistry 1 Department of Chemistry Lund University PO Box 124 S-221 00 Lund Sweden ; #======================================================================= data_[1] _audit_creation_method SHELXL-97 _chemical_name_systematic ; Diaquodibromodioxomolybdenum(VI) dihydrate 18-crown-6 ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H32 Br2 Mo O12' _chemical_formula_weight 624.14 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 8.66900(10) _cell_length_b 19.7867(2) _cell_length_c 13.53290(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.2840(10) _cell_angle_gamma 90.00 _cell_volume 2314.82(4) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 7325 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27.5 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 4.069 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.2012 _exptl_absorpt_correction_T_max 0.3144 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'Area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10949 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_sigmaI/netI 0.0135 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2567 _reflns_number_gt 2445 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-93 Sheldrick, (1993)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-93' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+6.2050P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00253(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2567 _refine_ls_number_parameters 142 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0632 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo 0.0000 0.206066(15) 0.2500 0.03197(10) Uani 1 d S . . Br Br 0.28729(3) 0.185476(15) 0.28356(3) 0.04980(12) Uani 1 d . . . O2 O 0.0212(2) 0.11836(10) 0.15153(14) 0.0397(4) Uani 1 d D . . H2C H 0.087(3) 0.1173(17) 0.110(2) 0.048 Uiso 1 d D . . H2D H -0.036(3) 0.0843(12) 0.145(2) 0.048 Uiso 1 d D . . O3 O -0.0164(2) 0.25927(11) 0.34679(19) 0.0577(6) Uani 1 d . . . O1 O 0.0531(2) -0.11333(10) 0.10700(15) 0.0421(4) Uani 1 d . . . C2 C 0.2156(4) -0.12545(17) 0.1154(2) 0.0511(7) Uani 1 d . . . H2A H 0.2481(9) -0.1376(4) 0.0532(16) 0.061 Uiso 1 calc R . . H2B H 0.2379(7) -0.1615(10) 0.1592(11) 0.061 Uiso 1 calc R . . C3 C 0.3015(4) -0.06409(18) 0.1522(2) 0.0524(8) Uani 1 d . . . H3A H 0.2511(13) -0.0450(5) 0.2078(15) 0.063 Uiso 1 calc R . . H3B H 0.406(3) -0.0767(4) 0.1758(7) 0.063 Uiso 1 calc R . . O4 O 0.3068(2) -0.01501(10) 0.07684(14) 0.0407(4) Uani 1 d . . . C5 C 0.3922(3) 0.04395(16) 0.1096(2) 0.0502(8) Uani 1 d . . . H5A H 0.496(3) 0.0323(3) 0.1262(5) 0.060 Uiso 1 calc R . . H5B H 0.3509(11) 0.0617(5) 0.1666(15) 0.060 Uiso 1 calc R . . C6 C 0.3835(3) 0.09529(16) 0.0302(3) 0.0498(8) Uani 1 d . . . H6A H 0.4487(17) 0.1329(10) 0.0493(5) 0.060 Uiso 1 calc R . . H6B H 0.4186(10) 0.0763(5) -0.0294(15) 0.060 Uiso 1 calc R . . O7 O 0.2278(2) 0.11723(10) 0.01308(14) 0.0388(4) Uani 1 d . . . C8 C 0.2002(4) 0.15836(15) -0.0731(2) 0.0487(7) Uani 1 d . . . H8A H 0.2335(9) 0.1343(6) -0.1316(15) 0.058 Uiso 1 calc R . . H8B H 0.2600(15) 0.2006(10) -0.0652(3) 0.058 Uiso 1 calc R . . C9 C 0.0317(4) 0.17409(15) -0.0874(2) 0.0478(7) Uani 1 d . . . H9A H -0.0028(10) 0.1959(6) -0.0272(15) 0.057 Uiso 1 calc R . . H9B H 0.0127(6) 0.2057(8) -0.1434(14) 0.057 Uiso 1 calc R . . O6 O -0.1340(2) 0.00678(10) 0.11334(15) 0.0423(4) Uani 1 d D . . H6C H -0.075(3) -0.0250(14) 0.110(3) 0.051 Uiso 1 d D . . H6D H -0.175(4) 0.0137(18) 0.0576(16) 0.051 Uiso 1 d 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 Mo 0.02553(15) 0.02459(16) 0.04697(19) 0.000 0.01063(12) 0.000 Br 0.02442(14) 0.04546(18) 0.0794(2) -0.02627(14) 0.00308(12) -0.00197(10) O2 0.0392(10) 0.0424(10) 0.0396(9) -0.0124(8) 0.0174(8) -0.0154(8) O3 0.0475(12) 0.0444(12) 0.0835(16) -0.0248(11) 0.0209(11) 0.0059(9) O1 0.0450(10) 0.0343(10) 0.0470(11) 0.0057(8) 0.0028(8) 0.0042(8) C2 0.0471(16) 0.0497(17) 0.0564(18) 0.0146(14) 0.0031(13) 0.0161(13) C3 0.0397(15) 0.073(2) 0.0430(15) 0.0059(15) -0.0061(12) 0.0108(14) O4 0.0343(9) 0.0464(11) 0.0403(10) -0.0077(8) -0.0037(7) 0.0019(8) C5 0.0275(12) 0.0574(18) 0.0638(19) -0.0299(16) -0.0081(12) 0.0074(12) C6 0.0252(12) 0.0474(16) 0.078(2) -0.0237(16) 0.0124(12) -0.0081(11) O7 0.0287(9) 0.0468(11) 0.0424(10) -0.0054(8) 0.0122(7) -0.0034(7) C8 0.0592(18) 0.0412(15) 0.0483(16) 0.0008(13) 0.0216(14) -0.0183(13) C9 0.069(2) 0.0314(13) 0.0441(15) 0.0090(11) 0.0087(14) -0.0010(13) O6 0.0456(11) 0.0369(10) 0.0441(10) -0.0065(9) 0.0017(9) -0.0039(8) _geom_special_details ; ? ; 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 Mo O3 1.695(2) . y Mo O3 1.695(2) 2 ? Mo O2 2.2040(19) . y Mo O2 2.2040(19) 2 ? Mo Br 2.5310(3) . y Mo Br 2.5310(3) 2 ? O1 C9 1.424(4) 5 ? O1 C2 1.425(4) . ? C2 C3 1.491(5) . ? C3 O4 1.412(4) . ? O4 C5 1.434(3) . ? C5 C6 1.477(5) . ? C6 O7 1.421(3) . ? O7 C8 1.428(4) . ? C8 C9 1.492(5) . ? C9 O1 1.424(4) 5 ? 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 Mo O3 103.19(18) . 2 ? O3 Mo O2 166.42(10) . . ? O3 Mo O2 90.36(10) 2 . ? O3 Mo O2 90.36(10) . 2 ? O3 Mo O2 166.42(10) 2 2 ? O2 Mo O2 76.12(10) . 2 ? O3 Mo Br 95.70(8) . . ? O3 Mo Br 95.77(7) 2 . ? O2 Mo Br 81.73(5) . . ? O2 Mo Br 83.70(5) 2 . ? O3 Mo Br 95.77(7) . 2 ? O3 Mo Br 95.70(8) 2 2 ? O2 Mo Br 83.70(5) . 2 ? O2 Mo Br 81.73(5) 2 2 ? Br Mo Br 161.473(19) . 2 ? C9 O1 C2 111.5(2) 5 . ? O1 C2 C3 110.8(3) . . ? O4 C3 C2 111.1(2) . . ? C3 O4 C5 112.4(2) . . ? O4 C5 C6 109.8(2) . . ? O7 C6 C5 108.9(2) . . ? C6 O7 C8 114.0(2) . . ? O7 C8 C9 109.1(2) . . ? O1 C9 C8 109.6(2) 5 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2C O7 0.831(18) 1.857(18) 2.687(2) 177(3) . O2 H2D O6 0.840(18) 1.789(19) 2.617(3) 169(3) . O6 H6C O1 0.812(18) 2.075(19) 2.882(3) 173(4) . O6 H6D O4 0.821(18) 2.076(19) 2.884(3) 168(3) 5 _refine_diff_density_max 1.157 _refine_diff_density_min -1.184 _refine_diff_density_rms 0.068 #==END data_[2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; Diaquodichlorodioxomolybdenum(VI) dihydrate 18-crown-6 ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H32 Cl2 Mo O12' _chemical_formula_weight 535.22 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.3364(2) _cell_length_b 19.2115(6) _cell_length_c 14.3430(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2297.10(11) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 6684 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.854 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.7717 _exptl_absorpt_correction_T_max 0.9348 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'Area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13297 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2026 _reflns_number_gt 1619 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-93 Sheldrick, (1993)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-93' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+2.9330P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0014(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2026 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.153 _refine_ls_shift/su_mean 0.013 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo 0.0000 0.20939(2) 0.2500 0.04733(19) Uani 1 d S . . Cl Cl 0.27793(11) 0.18788(5) 0.23162(8) 0.0647(3) Uani 1 d . . . O2 O 0.0174(3) 0.11862(17) 0.3442(2) 0.0669(8) Uani 1 d . . . H2A H -0.050(6) 0.089(2) 0.356(3) 0.080 Uiso 1 d . . . H2B H 0.081(6) 0.114(3) 0.378(3) 0.080 Uiso 1 d . . . O3 O 0.0222(4) 0.26346(17) 0.3409(2) 0.0870(10) Uani 1 d . . . O1 O 0.5193(5) 0.61640(17) 0.6028(2) 0.0848(10) Uani 1 d . . . O4 O 0.2596(4) 0.6138(2) 0.4743(3) 0.0833(10) Uani 1 d . . . O7 O 0.2060(4) 0.4788(2) 0.4101(2) 0.0881(10) Uani 1 d . . . C2 C 0.447(3) 0.6681(12) 0.5813(16) 0.122(10) Uani 0.50 d P A 1 H2A H 0.5038 0.6895 0.5289 0.147 Uiso 0.50 calc PR A 1 H2B H 0.4539 0.7006 0.6337 0.147 Uiso 0.50 calc PR A 1 C3 C 0.296(3) 0.6637(11) 0.5579(15) 0.069(6) Uani 0.50 d P A 1 H3C H 0.2571 0.7103 0.5419 0.083 Uiso 0.50 calc PR A 1 H3D H 0.2347 0.6477 0.6122 0.083 Uiso 0.50 calc PR A 1 C5 C 0.118(2) 0.5978(11) 0.4589(13) 0.089(6) Uani 0.50 d P A 1 H5A H 0.0576 0.6388 0.4388 0.106 Uiso 0.50 calc PR A 1 H5B H 0.0687 0.5795 0.5158 0.106 Uiso 0.50 calc PR A 1 C6 C 0.1161(17) 0.5488(8) 0.3912(15) 0.061(5) Uani 0.50 d P A 1 H6A H 0.1618 0.5695 0.3347 0.073 Uiso 0.50 calc PR A 1 H6B H 0.0037 0.5378 0.3776 0.073 Uiso 0.50 calc PR A 1 C2' C 0.428(4) 0.6790(6) 0.5682(15) 0.108(11) Uani 0.50 d P A 2 H2'1 H 0.4273 0.7154 0.6161 0.130 Uiso 0.50 calc PR A 2 H2'2 H 0.4796 0.6978 0.5123 0.130 Uiso 0.50 calc PR A 2 C3' C 0.235(3) 0.6547(14) 0.5429(17) 0.125(12) Uani 0.50 d P A 2 H3'1 H 0.1851 0.6304 0.5954 0.149 Uiso 0.50 calc PR A 2 H3'2 H 0.1693 0.6947 0.5250 0.149 Uiso 0.50 calc PR A 2 C5' C 0.0896(17) 0.5812(14) 0.440(2) 0.139(16) Uani 0.50 d P A 2 H5'1 H 0.0333 0.5604 0.4932 0.166 Uiso 0.50 calc PR A 2 H5'2 H 0.0217 0.6181 0.4141 0.166 Uiso 0.50 calc PR A 2 C6' C 0.122(3) 0.5238(10) 0.3633(18) 0.103(9) Uani 0.50 d P A 2 H6'1 H 0.0221 0.5034 0.3403 0.124 Uiso 0.50 calc PR A 2 H6'2 H 0.1833 0.5427 0.3107 0.124 Uiso 0.50 calc PR A 2 C8 C 0.2364(9) 0.4319(4) 0.3393(5) 0.126(3) Uani 1 d . . . H8A H 0.3043 0.4541 0.2921 0.151 Uiso 1 calc R . . H8B H 0.1350 0.4188 0.3095 0.151 Uiso 1 calc R . . C9 C 0.3167(8) 0.3690(4) 0.3743(5) 0.126(3) Uani 1 d . . . H9A H 0.2605 0.3520 0.4298 0.151 Uiso 1 calc R . . H9B H 0.3124 0.3325 0.3267 0.151 Uiso 1 calc R . . O5 O 0.3372(4) 0.48635(17) 0.5971(2) 0.0703(9) Uani 1 d . . . H6C H 0.313(6) 0.479(3) 0.545(3) 0.084 Uiso 1 d . . . H6D H 0.387(6) 0.517(3) 0.600(4) 0.084 Uiso 1 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 Mo 0.0462(3) 0.0397(3) 0.0561(3) 0.000 0.0048(2) 0.000 Cl 0.0437(5) 0.0629(6) 0.0874(7) 0.0156(5) 0.0052(4) -0.0026(4) O2 0.0580(18) 0.080(2) 0.0628(17) 0.0287(15) -0.0192(13) -0.0236(15) O3 0.075(2) 0.078(2) 0.108(2) -0.0451(19) 0.0179(17) -0.0239(17) O1 0.122(3) 0.0564(19) 0.076(2) -0.0108(16) 0.013(2) -0.002(2) O4 0.0549(19) 0.099(2) 0.096(2) 0.037(2) 0.0270(19) 0.0158(19) O7 0.079(2) 0.110(3) 0.075(2) 0.028(2) -0.0204(18) -0.034(2) C2 0.106(15) 0.18(2) 0.076(11) -0.047(13) 0.018(10) 0.051(14) C3 0.097(16) 0.048(7) 0.063(7) -0.017(6) 0.002(10) 0.025(9) C5 0.112(16) 0.065(8) 0.089(9) 0.031(7) -0.013(9) -0.019(9) C6 0.019(6) 0.055(11) 0.110(15) 0.026(9) -0.009(7) 0.005(6) C2' 0.24(3) 0.009(4) 0.076(10) -0.005(5) 0.030(15) -0.004(9) C3' 0.13(2) 0.118(18) 0.12(2) 0.057(14) 0.095(17) 0.095(16) C5' 0.010(5) 0.13(2) 0.28(4) 0.12(2) 0.051(12) 0.031(10) C6' 0.091(11) 0.106(18) 0.112(16) 0.066(14) -0.054(10) -0.057(12) C8 0.124(5) 0.157(7) 0.097(5) 0.018(5) -0.033(4) -0.070(5) C9 0.133(6) 0.115(5) 0.129(5) -0.053(4) 0.004(4) -0.067(5) O5 0.073(2) 0.065(2) 0.0724(19) 0.0169(17) -0.0003(17) 0.0052(15) _geom_special_details ; ? ; 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 Mo O3 1.677(3) . y Mo O3 1.677(3) 3 ? Mo O2 2.210(3) . y Mo O2 2.210(3) 3 ? Mo Cl 2.3682(9) . y Mo Cl 2.3682(9) 3 ? O1 C2 1.20(2) . ? O1 C9 1.434(7) 5_666 ? O1 C2' 1.51(2) . ? O4 C5 1.238(19) . ? O4 C3' 1.28(2) . ? O4 C3 1.564(18) . ? O4 C5' 1.63(3) . ? O7 C6' 1.30(2) . ? O7 C8 1.381(8) . ? O7 C6 1.564(16) . ? C2 C3 1.30(4) . ? C5 C6 1.35(3) . ? C2' C3' 1.71(4) . ? C5' C6' 1.58(4) . ? C8 C9 1.471(9) . ? C9 O1 1.434(7) 5_666 ? 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 Mo O3 103.5(3) . 3 ? O3 Mo O2 90.37(16) . . ? O3 Mo O2 166.12(16) 3 . ? O3 Mo O2 166.12(16) . 3 ? O3 Mo O2 90.37(16) 3 3 ? O2 Mo O2 75.83(17) . 3 ? O3 Mo Cl 94.98(11) . . ? O3 Mo Cl 97.43(10) 3 . ? O2 Mo Cl 82.31(8) . . ? O2 Mo Cl 81.87(8) 3 . ? O3 Mo Cl 97.43(10) . 3 ? O3 Mo Cl 94.98(11) 3 3 ? O2 Mo Cl 81.87(8) . 3 ? O2 Mo Cl 82.31(8) 3 3 ? Cl Mo Cl 159.90(5) . 3 ? C2 O1 C9 112.1(14) . 5_666 ? C2 O1 C2' 4.4(17) . . ? C9 O1 C2' 113.6(11) 5_666 . ? C5 O4 C3' 98.1(16) . . ? C5 O4 C3 118.2(14) . . ? C3' O4 C3 20.2(16) . . ? C5 O4 C5' 11.5(18) . . ? C3' O4 C5' 109.4(16) . . ? C3 O4 C5' 129.5(12) . . ? C6' O7 C8 98.8(11) . . ? C6' O7 C6 23.0(14) . . ? C8 O7 C6 121.4(8) . . ? O1 C2 C3 120(2) . . ? C2 C3 O4 115.1(15) . . ? O4 C5 C6 108.3(16) . . ? C5 C6 O7 117.9(15) . . ? C3' C2' O1 109.0(12) . . ? O4 C3' C2' 100.6(16) . . ? C6' C5' O4 109.2(11) . . ? O7 C6' C5' 101.4(19) . . ? O7 C8 C9 111.6(5) . . ? O1 C9 C8 110.6(5) 5_666 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2A O5 0.82(5) 1.85(5) 2.652(4) 165(5) 4_456 O2 H2B O4 0.73(5) 1.91(5) 2.636(4) 173(5) 8_655 O5 H6C O7 0.79(5) 2.12(5) 2.900(5) 166(5) . O5 H6D O1 0.73(5) 2.20(5) 2.925(5) 175(6) . _refine_diff_density_max 0.349 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.057 #==END data_[3] _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dichlorobis(methanol)dioxomolybdenum(VI) 18-crown-6 ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H32 Cl2 Mo O10' _chemical_formula_weight 527.24 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 8.71180(10) _cell_length_b 19.0183(3) _cell_length_c 13.6617(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.9490(10) _cell_angle_gamma 90.00 _cell_volume 2255.08(6) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 4704 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.862 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.7699 _exptl_absorpt_correction_T_max 0.8672 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'Area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6451 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2481 _reflns_number_gt 2191 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-93 Sheldrick, (1993)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-93' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+5.7273P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2481 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1335 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo 0.0000 0.30105(2) 0.2500 0.03884(18) Uani 1 d S . . Cl Cl 0.26842(11) 0.32184(6) 0.28066(9) 0.0562(3) Uani 1 d . . . O2 O 0.0175(3) 0.39333(15) 0.1496(2) 0.0408(6) Uani 1 d . . . H2A H 0.081(6) 0.393(3) 0.118(4) 0.049 Uiso 1 d . . . O3 O -0.0162(4) 0.24540(17) 0.3455(3) 0.0605(9) Uani 1 d . . . C1 C -0.0768(6) 0.4564(2) 0.1286(3) 0.0536(10) Uani 1 d . . . H1A H -0.1512 0.4473 0.0731 0.080 Uiso 1 calc R . . H1B H -0.0108 0.4952 0.1132 0.080 Uiso 1 calc R . . H1C H -0.1305 0.4682 0.1857 0.080 Uiso 1 calc R . . O1 O 0.3143(3) 0.51951(16) 0.07693(19) 0.0443(6) Uani 1 d . . . O4 O 0.2193(3) 0.38212(16) 0.0127(2) 0.0464(7) Uani 1 d . . . O7 O -0.0677(3) 0.38072(15) -0.1057(2) 0.0495(7) Uani 1 d . . . C2 C 0.3912(5) 0.4571(3) 0.1091(3) 0.0547(12) Uani 1 d . . . H2B H 0.3463 0.4389 0.1673 0.066 Uiso 1 calc R . . H2C H 0.5003 0.4672 0.1270 0.066 Uiso 1 calc R . . C3 C 0.3761(5) 0.4040(2) 0.0295(4) 0.0557(12) Uani 1 d . . . H3A H 0.4105 0.4242 -0.0309 0.067 Uiso 1 calc R . . H3B H 0.4414 0.3634 0.0479 0.067 Uiso 1 calc R . . C5 C 0.1894(6) 0.3410(3) -0.0744(3) 0.0568(12) Uani 1 d . . . H5A H 0.2541 0.2988 -0.0703 0.068 Uiso 1 calc R . . H5B H 0.2149 0.3683 -0.1317 0.068 Uiso 1 calc R . . C6 C 0.0246(6) 0.3205(2) -0.0860(3) 0.0549(11) Uani 1 d . . . H6A H 0.0072 0.2869 -0.1402 0.066 Uiso 1 calc R . . H6B H -0.0037 0.2978 -0.0258 0.066 Uiso 1 calc R . . C8 C -0.2280(5) 0.3647(3) -0.1138(4) 0.0597(12) Uani 1 d . . . H8A H -0.2600 0.3507 -0.0495 0.072 Uiso 1 calc R . . H8B H -0.2491 0.3255 -0.1596 0.072 Uiso 1 calc R . . C9 C -0.3158(5) 0.4288(3) -0.1503(3) 0.0585(12) Uani 1 d . . . H9A H -0.2696 0.4478 -0.2076 0.070 Uiso 1 calc R . . H9B H -0.4225 0.4157 -0.1709 0.070 Uiso 1 calc R . . 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 Mo 0.0346(3) 0.0292(2) 0.0552(3) 0.000 0.01831(19) 0.000 Cl 0.0357(5) 0.0506(6) 0.0837(8) 0.0271(5) 0.0129(5) 0.0060(4) O2 0.0415(15) 0.0435(15) 0.0398(14) 0.0046(11) 0.0172(11) 0.0085(12) O3 0.0598(19) 0.0435(16) 0.083(2) 0.0223(16) 0.0329(16) -0.0015(14) C1 0.061(3) 0.051(2) 0.050(2) 0.0003(19) 0.012(2) 0.006(2) O1 0.0407(14) 0.0497(16) 0.0412(14) 0.0078(12) -0.0036(11) 0.0006(12) O4 0.0384(14) 0.0541(17) 0.0492(16) -0.0006(13) 0.0179(12) 0.0005(12) O7 0.0521(17) 0.0378(14) 0.0589(17) -0.0077(13) 0.0063(13) -0.0053(13) C2 0.0322(19) 0.066(3) 0.064(3) 0.028(2) -0.0039(18) -0.0085(19) C3 0.035(2) 0.048(2) 0.087(3) 0.019(2) 0.020(2) 0.0089(17) C5 0.067(3) 0.057(3) 0.050(2) -0.008(2) 0.024(2) 0.021(2) C6 0.077(3) 0.036(2) 0.052(2) -0.0162(18) 0.009(2) 0.003(2) C8 0.055(3) 0.056(3) 0.068(3) -0.021(2) 0.005(2) -0.018(2) C9 0.045(2) 0.082(3) 0.047(2) -0.009(2) -0.0066(18) -0.011(2) _geom_special_details ; ? ; 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 Mo O3 1.696(3) 2 ? Mo O3 1.696(3) . y Mo O2 2.240(3) 2 ? Mo O2 2.240(3) . y Mo Cl 2.3730(10) 2 ? Mo Cl 2.3730(10) . y O2 C1 1.467(5) . ? O1 C9 1.404(6) 5_565 ? O1 C2 1.413(5) . ? O4 C3 1.428(5) . ? O4 C5 1.429(5) . ? O7 C6 1.411(5) . ? O7 C8 1.424(5) . ? C2 C3 1.482(7) . ? C5 C6 1.483(7) . ? C8 C9 1.502(7) . ? C9 O1 1.404(6) 5_565 ? 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 Mo O3 102.8(2) 2 . ? O3 Mo O2 167.05(14) 2 2 ? O3 Mo O2 90.18(14) . 2 ? O3 Mo O2 90.18(14) 2 . ? O3 Mo O2 167.05(14) . . ? O2 Mo O2 76.87(14) 2 . ? O3 Mo Cl 96.58(12) 2 2 ? O3 Mo Cl 95.36(12) . 2 ? O2 Mo Cl 81.93(8) 2 2 ? O2 Mo Cl 83.07(8) . 2 ? O3 Mo Cl 95.36(12) 2 . ? O3 Mo Cl 96.58(12) . . ? O2 Mo Cl 83.07(8) 2 . ? O2 Mo Cl 81.93(8) . . ? Cl Mo Cl 160.81(6) 2 . ? C1 O2 Mo 133.9(2) . . ? C9 O1 C2 113.0(3) 5_565 . ? C3 O4 C5 113.3(3) . . ? C6 O7 C8 112.3(4) . . ? O1 C2 C3 109.5(3) . . ? O4 C3 C2 109.8(3) . . ? O4 C5 C6 109.7(3) . . ? O7 C6 C5 109.7(4) . . ? O7 C8 C9 108.6(4) . . ? O1 C9 C8 111.0(3) 5_565 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2A O4 0.73(5) 1.97(5) 2.684(4) 167(5) . _refine_diff_density_max 1.453 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.090 #==END