Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2002 data_am75sa _database_code_CSD 175187 _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Livage, Carine' 'Ferey, Gerard' 'Hynaux, Amelie' 'Marrot, Jerome' 'Nogues, M.' _publ_contact_author_name 'Carine Livage' _publ_contact_author_address ; Institut Lavoisier, UMR CNRS 86 37 Universite de Versailles-St Quentin 45 Avenue des Etats-Unis Versailles 78035 Cedex FRANCE ; _publ_contact_author_email 'LIVAGE@CHIMIE.UVSQ.FR' _publ_section_title ; Solution process for the synthesis of the "high-pressure" phase CoMoO4 and X-ray single crystal resolution ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'CoMoO4-II' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Co Mo O4' _chemical_formula_weight 218.87 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 '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 P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 4.6598(7) _cell_length_b 5.6862(9) _cell_length_c 4.9159(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.521(3) _cell_angle_gamma 90.00 _cell_volume 130.25(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelepiped _exptl_crystal_colour black _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 202 _exptl_absorpt_coefficient_mu 10.964 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 893 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 29.85 _reflns_number_total 349 _reflns_number_observed 305 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc 'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.0000P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0621(71) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 349 _refine_ls_number_parameters 30 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_obs 0.0270 _refine_ls_wR_factor_all 0.0687 _refine_ls_wR_factor_obs 0.0660 _refine_ls_goodness_of_fit_all 1.050 _refine_ls_goodness_of_fit_obs 1.086 _refine_ls_restrained_S_all 1.050 _refine_ls_restrained_S_obs 1.086 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo Mo 0.0000 0.18500(9) 0.2500 0.0075(3) Uani 1 d S . Co Co 0.5000 0.67338(14) 0.2500 0.0092(3) Uani 1 d S . O1 O 0.2179(6) -0.1072(6) 0.0646(6) 0.0095(7) Uani 1 d . . O2 O 0.2551(6) 0.3772(5) 0.1021(6) 0.0103(7) Uani 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 0.0080(3) 0.0075(3) 0.0069(3) 0.000 0.0010(2) 0.000 Co 0.0089(5) 0.0104(5) 0.0083(5) 0.000 0.0000(3) 0.000 O1 0.010(2) 0.0100(14) 0.008(2) 0.0004(10) 0.0007(13) 0.0030(11) O2 0.0103(15) 0.0106(14) 0.010(2) -0.0006(11) 0.0013(12) -0.0010(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O2 1.775(3) 2 ? Mo O2 1.775(3) . ? Mo O1 1.895(3) 4_556 ? Mo O1 1.895(3) 3 ? Mo O1 2.154(3) 2 ? Mo O1 2.154(3) . ? Co O1 2.023(3) 2_665 ? Co O1 2.023(3) 1_565 ? Co O2 2.101(3) 4_566 ? Co O2 2.101(3) 3_665 ? Co O2 2.157(3) . ? Co O2 2.157(3) 2_655 ? O1 Mo 1.895(3) 3 ? O1 Co 2.023(3) 1_545 ? O2 Co 2.101(3) 3_665 ? 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 O2 Mo O2 104.0(2) 2 . ? O2 Mo O1 99.50(13) 2 4_556 ? O2 Mo O1 97.02(13) . 4_556 ? O2 Mo O1 97.02(13) 2 3 ? O2 Mo O1 99.50(13) . 3 ? O1 Mo O1 153.0(2) 4_556 3 ? O2 Mo O1 88.94(13) 2 2 ? O2 Mo O1 165.49(13) . 2 ? O1 Mo O1 74.08(13) 4_556 2 ? O1 Mo O1 85.08(10) 3 2 ? O2 Mo O1 165.49(13) 2 . ? O2 Mo O1 88.94(13) . . ? O1 Mo O1 85.08(10) 4_556 . ? O1 Mo O1 74.08(13) 3 . ? O1 Mo O1 79.0(2) 2 . ? O1 Co O1 103.9(2) 2_665 1_565 ? O1 Co O2 93.95(12) 2_665 4_566 ? O1 Co O2 95.73(12) 1_565 4_566 ? O1 Co O2 95.73(12) 2_665 3_665 ? O1 Co O2 93.95(12) 1_565 3_665 ? O2 Co O2 164.3(2) 4_566 3_665 ? O1 Co O2 166.63(13) 2_665 . ? O1 Co O2 89.43(12) 1_565 . ? O2 Co O2 83.19(10) 4_566 . ? O2 Co O2 84.55(12) 3_665 . ? O1 Co O2 89.43(12) 2_665 2_655 ? O1 Co O2 166.63(13) 1_565 2_655 ? O2 Co O2 84.55(12) 4_566 2_655 ? O2 Co O2 83.19(10) 3_665 2_655 ? O2 Co O2 77.3(2) . 2_655 ? Mo O1 Co 124.4(2) 3 1_545 ? Mo O1 Mo 105.92(13) 3 . ? Co O1 Mo 126.30(15) 1_545 . ? Mo O2 Co 128.6(2) . 3_665 ? Mo O2 Co 134.2(2) . . ? Co O2 Co 95.45(12) 3_665 . ? _refine_diff_density_max 1.371 _refine_diff_density_min -1.243 _refine_diff_density_rms 0.384