# ic020596m.cif CaMg2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'CaMg2' _chemical_formula_weight 88.7 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P 63/m m c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 6.2613(5) _cell_length_b 6.2613(5) _cell_length_c 10.1573(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 344.85(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 11.9 _cell_measurement_theta_max 43.1 _exptl_crystal_description irregular shape _exptl_crystal_colour silver _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.854 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 88 _exptl_absorpt_coefficient_mu 0.940 _exptl_absorpt_correction_type numerical (X-shape, (Stoe & Cie, 1997)) _exptl_absorpt_correction_T_min 0.6658 _exptl_absorpt_correction_T_max 0.8045 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Stoe IPDS (version 2.87) _diffrn_measurement_method f scan _diffrn_detector_area_resol_mean area detector _diffrn_standards_interval_count 6.0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3024 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0105 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 27.93 _reflns_number_total 189 _reflns_number_gt 155 _reflns_threshold_expression >2sigma(I) _computing_data_collection EXPOSE in IPDS (Stoe & Cie, 1997) _computing_cell_refinement PIRUM (Werner & Ericsson, 1993) _computing_data_reduction X-RED (Stoe & Cie, 1997) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Atoms (Dowty, 1997) _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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. Unit cell parameters least square refined from 31 measured and indexed lines of a Guinier powder diagram (Cuka, Si (NIST) standard) (program PIRUM (Werner & Ericsson, 1993)) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0134P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 189 _refine_ls_number_parameters 10 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0150 _refine_ls_R_factor_gt 0.0109 _refine_ls_wR_factor_ref 0.0238 _refine_ls_wR_factor_gt 0.0233 _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_restrained_S_all 1.187 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.3333 0.6667 0.06190(3) 0.01512(11) Uani 1 6 d S . . Mg1 Mg 0.0000 0.0000 0.0000 0.01524(16) Uani 1 12 d S . . Mg2 Mg 0.83129(4) 0.66258(8) 0.2500 0.01502(13) Uani 1 4 d S . . 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 Ca1 0.01530(13) 0.01530(13) 0.01475(15) 0.000 0.000 0.00765(7) Mg1 0.0170(2) 0.0170(2) 0.0117(3) 0.000 0.000 0.00851(11) Mg2 0.0162(2) 0.0119(2) 0.01553(18) 0.000 0.000 0.00594(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 Ca1 Mg2 3.6365(4) 15 ? Ca1 Mg2 3.6365(4) 13_665 ? Ca1 Mg2 3.6365(4) 14_565 ? Ca1 Mg2 3.6677(3) 2_665 ? Ca1 Mg2 3.6677(3) 3_565 ? Ca1 Mg2 3.6677(3) . ? Ca1 Mg2 3.6677(3) 3_675 ? Ca1 Mg2 3.6677(3) 1_455 ? Ca1 Mg2 3.6677(3) 2_655 ? Ca1 Mg1 3.6692(3) 1_565 ? Ca1 Mg1 3.6692(3) . ? Ca1 Mg1 3.6692(3) 1_665 ? Mg1 Mg2 3.1298(3) 14_455 ? Mg1 Mg2 3.1298(3) 2_655 ? Mg1 Mg2 3.1298(3) 15_545 ? Mg1 Mg2 3.1298(3) 3_565 ? Mg1 Mg2 3.1298(3) 13_665 ? Mg1 Mg2 3.1298(3) 1_445 ? Mg1 Ca1 3.6692(3) 1_545 ? Mg1 Ca1 3.6692(3) 13_565 ? Mg1 Ca1 3.6692(3) 13 ? Mg1 Ca1 3.6692(3) 1_445 ? Mg1 Ca1 3.6692(3) 13_665 ? Mg2 Mg2 3.0923(8) 2_655 ? Mg2 Mg2 3.0923(8) 3_665 ? Mg2 Mg1 3.1298(3) 4_665 ? Mg2 Mg1 3.1298(3) 1_665 ? Mg2 Mg2 3.1690(8) 2_765 ? Mg2 Mg2 3.1690(8) 3_675 ? Mg2 Ca1 3.6365(4) 13_665 ? Mg2 Ca1 3.6365(4) 4_665 ? Mg2 Ca1 3.6677(3) 16_656 ? Mg2 Ca1 3.6677(3) 16_556 ? Mg2 Ca1 3.6677(3) 1_655 ? 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 Mg2 Ca1 Mg2 50.324(11) 15 13_665 ? Mg2 Ca1 Mg2 50.324(11) 15 14_565 ? Mg2 Ca1 Mg2 50.324(11) 13_665 14_565 ? Mg2 Ca1 Mg2 95.300(9) 15 2_665 ? Mg2 Ca1 Mg2 144.908(5) 13_665 2_665 ? Mg2 Ca1 Mg2 116.799(5) 14_565 2_665 ? Mg2 Ca1 Mg2 116.799(5) 15 3_565 ? Mg2 Ca1 Mg2 95.300(9) 13_665 3_565 ? Mg2 Ca1 Mg2 144.908(5) 14_565 3_565 ? Mg2 Ca1 Mg2 95.334(6) 2_665 3_565 ? Mg2 Ca1 Mg2 144.908(5) 15 . ? Mg2 Ca1 Mg2 116.799(5) 13_665 . ? Mg2 Ca1 Mg2 95.300(9) 14_565 . ? Mg2 Ca1 Mg2 95.334(6) 2_665 . ? Mg2 Ca1 Mg2 95.334(6) 3_565 . ? Mg2 Ca1 Mg2 116.799(5) 15 3_675 ? Mg2 Ca1 Mg2 144.908(5) 13_665 3_675 ? Mg2 Ca1 Mg2 95.300(9) 14_565 3_675 ? Mg2 Ca1 Mg2 49.867(13) 2_665 3_675 ? Mg2 Ca1 Mg2 117.207(9) 3_565 3_675 ? Mg2 Ca1 Mg2 51.191(13) . 3_675 ? Mg2 Ca1 Mg2 95.300(9) 15 1_455 ? Mg2 Ca1 Mg2 116.799(5) 13_665 1_455 ? Mg2 Ca1 Mg2 144.908(5) 14_565 1_455 ? Mg2 Ca1 Mg2 51.191(13) 2_665 1_455 ? Mg2 Ca1 Mg2 49.867(13) 3_565 1_455 ? Mg2 Ca1 Mg2 117.207(9) . 1_455 ? Mg2 Ca1 Mg2 95.334(6) 3_675 1_455 ? Mg2 Ca1 Mg2 144.908(5) 15 2_655 ? Mg2 Ca1 Mg2 95.300(9) 13_665 2_655 ? Mg2 Ca1 Mg2 116.799(5) 14_565 2_655 ? Mg2 Ca1 Mg2 117.207(9) 2_665 2_655 ? Mg2 Ca1 Mg2 51.191(13) 3_565 2_655 ? Mg2 Ca1 Mg2 49.867(13) . 2_655 ? Mg2 Ca1 Mg2 95.334(6) 3_675 2_655 ? Mg2 Ca1 Mg2 95.334(6) 1_455 2_655 ? Mg2 Ca1 Mg1 50.730(6) 15 1_565 ? Mg2 Ca1 Mg1 95.311(6) 13_665 1_565 ? Mg2 Ca1 Mg1 95.311(6) 14_565 1_565 ? Mg2 Ca1 Mg1 50.502(5) 2_665 1_565 ? Mg2 Ca1 Mg1 94.779(7) 3_565 1_565 ? Mg2 Ca1 Mg1 145.137(7) . 1_565 ? Mg2 Ca1 Mg1 94.779(7) 3_675 1_565 ? Mg2 Ca1 Mg1 50.502(5) 1_455 1_565 ? Mg2 Ca1 Mg1 145.138(7) 2_655 1_565 ? Mg2 Ca1 Mg1 95.311(6) 15 . ? Mg2 Ca1 Mg1 50.730(6) 13_665 . ? Mg2 Ca1 Mg1 95.311(6) 14_565 . ? Mg2 Ca1 Mg1 145.138(7) 2_665 . ? Mg2 Ca1 Mg1 50.502(5) 3_565 . ? Mg2 Ca1 Mg1 94.779(7) . . ? Mg2 Ca1 Mg1 145.138(7) 3_675 . ? Mg2 Ca1 Mg1 94.779(7) 1_455 . ? Mg2 Ca1 Mg1 50.502(5) 2_655 . ? Mg1 Ca1 Mg1 117.126(2) 1_565 . ? Mg2 Ca1 Mg1 95.311(6) 15 1_665 ? Mg2 Ca1 Mg1 95.311(6) 13_665 1_665 ? Mg2 Ca1 Mg1 50.730(6) 14_565 1_665 ? Mg2 Ca1 Mg1 94.779(7) 2_665 1_665 ? Mg2 Ca1 Mg1 145.137(7) 3_565 1_665 ? Mg2 Ca1 Mg1 50.502(5) . 1_665 ? Mg2 Ca1 Mg1 50.502(5) 3_675 1_665 ? Mg2 Ca1 Mg1 145.137(7) 1_455 1_665 ? Mg2 Ca1 Mg1 94.779(7) 2_655 1_665 ? Mg1 Ca1 Mg1 117.126(2) 1_565 1_665 ? Mg1 Ca1 Mg1 117.126(2) . 1_665 ? Mg2 Mg1 Mg2 180.000(9) 14_455 2_655 ? Mg2 Mg1 Mg2 60.830(12) 14_455 15_545 ? Mg2 Mg1 Mg2 119.170(12) 2_655 15_545 ? Mg2 Mg1 Mg2 119.170(12) 14_455 3_565 ? Mg2 Mg1 Mg2 60.830(12) 2_655 3_565 ? Mg2 Mg1 Mg2 180.000(8) 15_545 3_565 ? Mg2 Mg1 Mg2 60.830(12) 14_455 13_665 ? Mg2 Mg1 Mg2 119.170(12) 2_655 13_665 ? Mg2 Mg1 Mg2 60.830(12) 15_545 13_665 ? Mg2 Mg1 Mg2 119.170(12) 3_565 13_665 ? Mg2 Mg1 Mg2 119.170(12) 14_455 1_445 ? Mg2 Mg1 Mg2 60.830(12) 2_655 1_445 ? Mg2 Mg1 Mg2 119.170(12) 15_545 1_445 ? Mg2 Mg1 Mg2 60.830(12) 3_565 1_445 ? Mg2 Mg1 Mg2 180.000(15) 13_665 1_445 ? Mg2 Mg1 Ca1 115.277(4) 14_455 1_545 ? Mg2 Mg1 Ca1 64.723(4) 2_655 1_545 ? Mg2 Mg1 Ca1 64.093(9) 15_545 1_545 ? Mg2 Mg1 Ca1 115.907(9) 3_565 1_545 ? Mg2 Mg1 Ca1 115.277(4) 13_665 1_545 ? Mg2 Mg1 Ca1 64.723(4) 1_445 1_545 ? Mg2 Mg1 Ca1 64.723(4) 14_455 13_565 ? Mg2 Mg1 Ca1 115.277(4) 2_655 13_565 ? Mg2 Mg1 Ca1 115.907(9) 15_545 13_565 ? Mg2 Mg1 Ca1 64.093(9) 3_565 13_565 ? Mg2 Mg1 Ca1 64.723(4) 13_665 13_565 ? Mg2 Mg1 Ca1 115.277(4) 1_445 13_565 ? Ca1 Mg1 Ca1 180.0 1_545 13_565 ? Mg2 Mg1 Ca1 115.277(4) 14_455 . ? Mg2 Mg1 Ca1 64.723(4) 2_655 . ? Mg2 Mg1 Ca1 115.277(4) 15_545 . ? Mg2 Mg1 Ca1 64.723(4) 3_565 . ? Mg2 Mg1 Ca1 64.093(9) 13_665 . ? Mg2 Mg1 Ca1 115.907(9) 1_445 . ? Ca1 Mg1 Ca1 117.126(2) 1_545 . ? Ca1 Mg1 Ca1 62.874(2) 13_565 . ? Mg2 Mg1 Ca1 64.723(4) 14_455 13 ? Mg2 Mg1 Ca1 115.277(4) 2_655 13 ? Mg2 Mg1 Ca1 64.723(4) 15_545 13 ? Mg2 Mg1 Ca1 115.277(4) 3_565 13 ? Mg2 Mg1 Ca1 115.907(9) 13_665 13 ? Mg2 Mg1 Ca1 64.093(9) 1_445 13 ? Ca1 Mg1 Ca1 62.874(2) 1_545 13 ? Ca1 Mg1 Ca1 117.126(2) 13_565 13 ? Ca1 Mg1 Ca1 180.0 . 13 ? Mg2 Mg1 Ca1 64.093(9) 14_455 1_445 ? Mg2 Mg1 Ca1 115.907(9) 2_655 1_445 ? Mg2 Mg1 Ca1 115.277(4) 15_545 1_445 ? Mg2 Mg1 Ca1 64.723(4) 3_565 1_445 ? Mg2 Mg1 Ca1 115.277(4) 13_665 1_445 ? Mg2 Mg1 Ca1 64.723(4) 1_445 1_445 ? Ca1 Mg1 Ca1 117.126(2) 1_545 1_445 ? Ca1 Mg1 Ca1 62.874(2) 13_565 1_445 ? Ca1 Mg1 Ca1 117.126(2) . 1_445 ? Ca1 Mg1 Ca1 62.874(2) 13 1_445 ? Mg2 Mg1 Ca1 115.907(9) 14_455 13_665 ? Mg2 Mg1 Ca1 64.093(9) 2_655 13_665 ? Mg2 Mg1 Ca1 64.723(4) 15_545 13_665 ? Mg2 Mg1 Ca1 115.277(4) 3_565 13_665 ? Mg2 Mg1 Ca1 64.723(4) 13_665 13_665 ? Mg2 Mg1 Ca1 115.277(4) 1_445 13_665 ? Ca1 Mg1 Ca1 62.874(2) 1_545 13_665 ? Ca1 Mg1 Ca1 117.126(2) 13_565 13_665 ? Ca1 Mg1 Ca1 62.874(2) . 13_665 ? Ca1 Mg1 Ca1 117.126(2) 13 13_665 ? Ca1 Mg1 Ca1 180.0 1_445 13_665 ? Mg2 Mg2 Mg2 60.0 2_655 3_665 ? Mg2 Mg2 Mg1 120.415(6) 2_655 4_665 ? Mg2 Mg2 Mg1 120.415(6) 3_665 4_665 ? Mg2 Mg2 Mg1 120.415(6) 2_655 1_665 ? Mg2 Mg2 Mg1 120.415(6) 3_665 1_665 ? Mg1 Mg2 Mg1 108.453(14) 4_665 1_665 ? Mg2 Mg2 Mg2 180.000(15) 2_655 2_765 ? Mg2 Mg2 Mg2 120.0 3_665 2_765 ? Mg1 Mg2 Mg2 59.585(6) 4_665 2_765 ? Mg1 Mg2 Mg2 59.585(6) 1_665 2_765 ? Mg2 Mg2 Mg2 120.0 2_655 3_675 ? Mg2 Mg2 Mg2 180.000(15) 3_665 3_675 ? Mg1 Mg2 Mg2 59.585(6) 4_665 3_675 ? Mg1 Mg2 Mg2 59.585(6) 1_665 3_675 ? Mg2 Mg2 Mg2 60.0 2_765 3_675 ? Mg2 Mg2 Ca1 64.838(6) 2_655 13_665 ? Mg2 Mg2 Ca1 64.838(6) 3_665 13_665 ? Mg1 Mg2 Ca1 173.630(12) 4_665 13_665 ? Mg1 Mg2 Ca1 65.177(7) 1_665 13_665 ? Mg2 Mg2 Ca1 115.162(6) 2_765 13_665 ? Mg2 Mg2 Ca1 115.162(6) 3_675 13_665 ? Mg2 Mg2 Ca1 64.838(6) 2_655 4_665 ? Mg2 Mg2 Ca1 64.838(6) 3_665 4_665 ? Mg1 Mg2 Ca1 65.177(7) 4_665 4_665 ? Mg1 Mg2 Ca1 173.630(12) 1_665 4_665 ? Mg2 Mg2 Ca1 115.162(6) 2_765 4_665 ? Mg2 Mg2 Ca1 115.162(6) 3_675 4_665 ? Ca1 Mg2 Ca1 121.193(14) 13_665 4_665 ? Mg2 Mg2 Ca1 65.067(6) 2_655 . ? Mg2 Mg2 Ca1 115.596(6) 3_665 . ? Mg1 Mg2 Ca1 114.779(8) 4_665 . ? Mg1 Mg2 Ca1 64.775(5) 1_665 . ? Mg2 Mg2 Ca1 114.933(6) 2_765 . ? Mg2 Mg2 Ca1 64.404(6) 3_675 . ? Ca1 Mg2 Ca1 63.201(5) 13_665 . ? Ca1 Mg2 Ca1 117.180(7) 4_665 . ? Mg2 Mg2 Ca1 115.596(6) 2_655 16_656 ? Mg2 Mg2 Ca1 65.067(6) 3_665 16_656 ? Mg1 Mg2 Ca1 64.775(5) 4_665 16_656 ? Mg1 Mg2 Ca1 114.779(8) 1_665 16_656 ? Mg2 Mg2 Ca1 64.404(6) 2_765 16_656 ? Mg2 Mg2 Ca1 114.933(6) 3_675 16_656 ? Ca1 Mg2 Ca1 117.180(7) 13_665 16_656 ? Ca1 Mg2 Ca1 63.201(5) 4_665 16_656 ? Ca1 Mg2 Ca1 179.308(13) . 16_656 ? Mg2 Mg2 Ca1 65.067(6) 2_655 16_556 ? Mg2 Mg2 Ca1 115.596(6) 3_665 16_556 ? Mg1 Mg2 Ca1 64.775(5) 4_665 16_556 ? Mg1 Mg2 Ca1 114.779(8) 1_665 16_556 ? Mg2 Mg2 Ca1 114.933(6) 2_765 16_556 ? Mg2 Mg2 Ca1 64.404(6) 3_675 16_556 ? Ca1 Mg2 Ca1 117.180(7) 13_665 16_556 ? Ca1 Mg2 Ca1 63.201(5) 4_665 16_556 ? Ca1 Mg2 Ca1 62.788(9) . 16_556 ? Ca1 Mg2 Ca1 117.207(9) 16_656 16_556 ? Mg2 Mg2 Ca1 115.596(6) 2_655 1_655 ? Mg2 Mg2 Ca1 65.067(6) 3_665 1_655 ? Mg1 Mg2 Ca1 114.779(8) 4_665 1_655 ? Mg1 Mg2 Ca1 64.775(5) 1_665 1_655 ? Mg2 Mg2 Ca1 64.404(6) 2_765 1_655 ? Mg2 Mg2 Ca1 114.933(6) 3_675 1_655 ? Ca1 Mg2 Ca1 63.201(5) 13_665 1_655 ? Ca1 Mg2 Ca1 117.180(7) 4_665 1_655 ? Ca1 Mg2 Ca1 117.207(9) . 1_655 ? Ca1 Mg2 Ca1 62.788(9) 16_656 1_655 ? Ca1 Mg2 Ca1 179.308(13) 16_556 1_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.93 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.221 _refine_diff_density_min -0.168 _refine_diff_density_rms 0.038 #===END CaAl0.44Mg1.56 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum CaAl0.44Mg1.56 _chemical_formula_weight 89.7 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P 63/m m c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 6.0755(4) _cell_length_b 6.0755(4) _cell_length_c 9.7708(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 312.34(4) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 12.4 _cell_measurement_theta_max 40.4 _exptl_crystal_description irregular shape _exptl_crystal_colour silver _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.872 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 267 _exptl_absorpt_coefficient_mu 3.173 _exptl_absorpt_correction_type numerical (X-shape, (Stoe & Cie, 1997)) _exptl_absorpt_correction_T_min 0.6948 _exptl_absorpt_correction_T_max 0.7724 _exptl_absorpt_process_details ? _exptl_special_details ? ; _diffrn_ambient_temperature 293(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 Stoe IPDS (version 2.87) _diffrn_measurement_method f scan _diffrn_detector_area_resol_mean area detector _diffrn_standards_number 6.0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2750 _diffrn_reflns_av_R_equivalents 0.0733 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.87 _diffrn_reflns_theta_max 28.05 _reflns_number_total 171 _reflns_number_gt 125 _reflns_threshold_expression >2sigma(I) _computing_data_collection EXPOSE in IPDS (Stoe & Cie, 1997) _computing_cell_refinement PIRUM (Werner & Ericsson, 1993) _computing_data_reduction X-RED (Stoe & Cie, 1997) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Atoms (Dowty, 1997) _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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. Unit cell parameters least square refined from 23 measured and indexed lines of a Guinier powder diagram (Cuka, Si (NIST) standard) (program PIRUM (Werner & Ericsson, 1993)) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 171 _refine_ls_number_parameters 10 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.1029 _refine_ls_wR_factor_gt 0.0478 _refine_ls_goodness_of_fit_ref 6.642 _refine_ls_restrained_S_all 6.642 _refine_ls_shift/su_max 0.000 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.3333 0.6667 0.0618(2) 0.0181(6) Uani 1 6 d S . . Mg1 Mg 0.0000 0.0000 0.0000 0.0152(12) Uani 1 12 d S . . AL Mg 0.8312(4) 0.6623(7) 0.2500 0.0154(8) Uani 1 4 d S . . 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 Ca1 0.0182(8) 0.0182(8) 0.0179(11) 0.000 0.000 0.0091(4) Mg1 0.0178(17) 0.0178(17) 0.010(3) 0.000 0.000 0.0089(9) AL 0.0181(13) 0.0127(15) 0.0136(12) 0.000 0.000 0.0064(7) _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 Ca1 AL 3.504(3) 13_665 ? Ca1 AL 3.504(3) 15 ? Ca1 AL 3.504(3) 14_565 ? Ca1 AL 3.5510(12) 3_675 ? Ca1 AL 3.5510(12) 2_665 ? Ca1 AL 3.5510(12) 1_455 ? Ca1 AL 3.5510(12) 3_565 ? Ca1 AL 3.5510(12) . ? Ca1 AL 3.5510(12) 2_655 ? Ca1 Mg1 3.5593(5) 1_565 ? Ca1 Mg1 3.5593(5) . ? Ca1 Mg1 3.5593(5) 1_665 ? Mg1 AL 3.020(2) 14_455 ? Mg1 AL 3.020(2) 2_655 ? Mg1 AL 3.020(2) 15_545 ? Mg1 AL 3.020(2) 3_565 ? Mg1 AL 3.020(2) 13_665 ? Mg1 AL 3.020(2) 1_445 ? Mg1 Ca1 3.5593(5) 1_545 ? Mg1 Ca1 3.5593(5) 13_565 ? Mg1 Ca1 3.5593(5) 13 ? Mg1 Ca1 3.5593(5) 13_665 ? Mg1 Ca1 3.5593(5) 1_445 ? AL AL 2.998(7) 2_655 ? AL AL 2.998(7) 3_665 ? AL Mg1 3.020(2) 4_665 ? AL Mg1 3.020(2) 1_665 ? AL AL 3.077(7) 2_765 ? AL AL 3.077(7) 3_675 ? AL Ca1 3.504(3) 13_665 ? AL Ca1 3.504(3) 4_665 ? AL Ca1 3.5510(12) 16_656 ? AL Ca1 3.5510(12) 1_655 ? AL Ca1 3.5510(12) 16_556 ? 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 AL Ca1 AL 50.66(10) 13_665 15 ? AL Ca1 AL 50.66(10) 13_665 14_565 ? AL Ca1 AL 50.66(10) 15 14_565 ? AL Ca1 AL 144.87(4) 13_665 3_675 ? AL Ca1 AL 116.56(3) 15 3_675 ? AL Ca1 AL 94.92(7) 14_565 3_675 ? AL Ca1 AL 144.87(4) 13_665 2_665 ? AL Ca1 AL 94.92(7) 15 2_665 ? AL Ca1 AL 116.56(3) 14_565 2_665 ? AL Ca1 AL 49.94(12) 3_675 2_665 ? AL Ca1 AL 116.56(3) 13_665 1_455 ? AL Ca1 AL 94.92(7) 15 1_455 ? AL Ca1 AL 144.87(4) 14_565 1_455 ? AL Ca1 AL 95.61(4) 3_675 1_455 ? AL Ca1 AL 51.35(12) 2_665 1_455 ? AL Ca1 AL 94.92(7) 13_665 3_565 ? AL Ca1 AL 116.56(3) 15 3_565 ? AL Ca1 AL 144.87(4) 14_565 3_565 ? AL Ca1 AL 117.62(6) 3_675 3_565 ? AL Ca1 AL 95.61(4) 2_665 3_565 ? AL Ca1 AL 49.94(12) 1_455 3_565 ? AL Ca1 AL 116.56(3) 13_665 . ? AL Ca1 AL 144.87(4) 15 . ? AL Ca1 AL 94.92(7) 14_565 . ? AL Ca1 AL 51.35(12) 3_675 . ? AL Ca1 AL 95.61(4) 2_665 . ? AL Ca1 AL 117.62(6) 1_455 . ? AL Ca1 AL 95.61(4) 3_565 . ? AL Ca1 AL 94.92(7) 13_665 2_655 ? AL Ca1 AL 144.87(4) 15 2_655 ? AL Ca1 AL 116.56(3) 14_565 2_655 ? AL Ca1 AL 95.61(4) 3_675 2_655 ? AL Ca1 AL 117.62(6) 2_665 2_655 ? AL Ca1 AL 95.61(4) 1_455 2_655 ? AL Ca1 AL 51.35(12) 3_565 2_655 ? AL Ca1 AL 49.94(12) . 2_655 ? AL Ca1 Mg1 95.50(5) 13_665 1_565 ? AL Ca1 Mg1 50.63(6) 15 1_565 ? AL Ca1 Mg1 95.50(5) 14_565 1_565 ? AL Ca1 Mg1 94.68(6) 3_675 1_565 ? AL Ca1 Mg1 50.28(4) 2_665 1_565 ? AL Ca1 Mg1 50.28(4) 1_455 1_565 ? AL Ca1 Mg1 94.68(6) 3_565 1_565 ? AL Ca1 Mg1 145.20(7) . 1_565 ? AL Ca1 Mg1 145.20(7) 2_655 1_565 ? AL Ca1 Mg1 50.63(6) 13_665 . ? AL Ca1 Mg1 95.50(5) 15 . ? AL Ca1 Mg1 95.50(5) 14_565 . ? AL Ca1 Mg1 145.20(7) 3_675 . ? AL Ca1 Mg1 145.20(7) 2_665 . ? AL Ca1 Mg1 94.68(7) 1_455 . ? AL Ca1 Mg1 50.28(4) 3_565 . ? AL Ca1 Mg1 94.68(6) . . ? AL Ca1 Mg1 50.28(4) 2_655 . ? Mg1 Ca1 Mg1 117.18(2) 1_565 . ? AL Ca1 Mg1 95.50(5) 13_665 1_665 ? AL Ca1 Mg1 95.50(5) 15 1_665 ? AL Ca1 Mg1 50.63(6) 14_565 1_665 ? AL Ca1 Mg1 50.28(4) 3_675 1_665 ? AL Ca1 Mg1 94.68(7) 2_665 1_665 ? AL Ca1 Mg1 145.20(7) 1_455 1_665 ? AL Ca1 Mg1 145.20(7) 3_565 1_665 ? AL Ca1 Mg1 50.28(4) . 1_665 ? AL Ca1 Mg1 94.68(6) 2_655 1_665 ? Mg1 Ca1 Mg1 117.18(2) 1_565 1_665 ? Mg1 Ca1 Mg1 117.18(2) . 1_665 ? AL Mg1 AL 180.00(15) 14_455 2_655 ? AL Mg1 AL 61.25(10) 14_455 15_545 ? AL Mg1 AL 118.75(10) 2_655 15_545 ? AL Mg1 AL 118.75(10) 14_455 3_565 ? AL Mg1 AL 61.25(10) 2_655 3_565 ? AL Mg1 AL 180.00(7) 15_545 3_565 ? AL Mg1 AL 61.25(10) 14_455 13_665 ? AL Mg1 AL 118.75(10) 2_655 13_665 ? AL Mg1 AL 61.25(10) 15_545 13_665 ? AL Mg1 AL 118.75(10) 3_565 13_665 ? AL Mg1 AL 118.75(10) 14_455 1_445 ? AL Mg1 AL 61.25(10) 2_655 1_445 ? AL Mg1 AL 118.75(10) 15_545 1_445 ? AL Mg1 AL 61.25(10) 3_565 1_445 ? AL Mg1 AL 180.00(15) 13_665 1_445 ? AL Mg1 Ca1 115.28(4) 14_455 1_545 ? AL Mg1 Ca1 64.72(4) 2_655 1_545 ? AL Mg1 Ca1 63.74(7) 15_545 1_545 ? AL Mg1 Ca1 116.26(7) 3_565 1_545 ? AL Mg1 Ca1 115.28(4) 13_665 1_545 ? AL Mg1 Ca1 64.72(4) 1_445 1_545 ? AL Mg1 Ca1 64.72(4) 14_455 13_565 ? AL Mg1 Ca1 115.28(4) 2_655 13_565 ? AL Mg1 Ca1 116.26(7) 15_545 13_565 ? AL Mg1 Ca1 63.74(7) 3_565 13_565 ? AL Mg1 Ca1 64.72(4) 13_665 13_565 ? AL Mg1 Ca1 115.28(4) 1_445 13_565 ? Ca1 Mg1 Ca1 180.0 1_545 13_565 ? AL Mg1 Ca1 64.72(4) 14_455 13 ? AL Mg1 Ca1 115.28(4) 2_655 13 ? AL Mg1 Ca1 64.72(4) 15_545 13 ? AL Mg1 Ca1 115.28(4) 3_565 13 ? AL Mg1 Ca1 116.26(7) 13_665 13 ? AL Mg1 Ca1 63.74(7) 1_445 13 ? Ca1 Mg1 Ca1 62.82(2) 1_545 13 ? Ca1 Mg1 Ca1 117.18(2) 13_565 13 ? AL Mg1 Ca1 115.28(4) 14_455 . ? AL Mg1 Ca1 64.72(4) 2_655 . ? AL Mg1 Ca1 115.28(4) 15_545 . ? AL Mg1 Ca1 64.72(4) 3_565 . ? AL Mg1 Ca1 63.74(7) 13_665 . ? AL Mg1 Ca1 116.26(7) 1_445 . ? Ca1 Mg1 Ca1 117.18(2) 1_545 . ? Ca1 Mg1 Ca1 62.82(2) 13_565 . ? Ca1 Mg1 Ca1 180.00(7) 13 . ? AL Mg1 Ca1 116.26(7) 14_455 13_665 ? AL Mg1 Ca1 63.74(7) 2_655 13_665 ? AL Mg1 Ca1 64.72(4) 15_545 13_665 ? AL Mg1 Ca1 115.28(4) 3_565 13_665 ? AL Mg1 Ca1 64.72(4) 13_665 13_665 ? AL Mg1 Ca1 115.28(4) 1_445 13_665 ? Ca1 Mg1 Ca1 62.82(2) 1_545 13_665 ? Ca1 Mg1 Ca1 117.18(2) 13_565 13_665 ? Ca1 Mg1 Ca1 117.18(2) 13 13_665 ? Ca1 Mg1 Ca1 62.82(2) . 13_665 ? AL Mg1 Ca1 63.74(7) 14_455 1_445 ? AL Mg1 Ca1 116.26(7) 2_655 1_445 ? AL Mg1 Ca1 115.28(4) 15_545 1_445 ? AL Mg1 Ca1 64.72(4) 3_565 1_445 ? AL Mg1 Ca1 115.28(4) 13_665 1_445 ? AL Mg1 Ca1 64.72(4) 1_445 1_445 ? Ca1 Mg1 Ca1 117.18(2) 1_545 1_445 ? Ca1 Mg1 Ca1 62.82(2) 13_565 1_445 ? Ca1 Mg1 Ca1 62.82(2) 13 1_445 ? Ca1 Mg1 Ca1 117.18(2) . 1_445 ? Ca1 Mg1 Ca1 180.0 13_665 1_445 ? AL AL AL 60.0 2_655 3_665 ? AL AL Mg1 120.62(5) 2_655 4_665 ? AL AL Mg1 120.62(5) 3_665 4_665 ? AL AL Mg1 120.62(5) 2_655 1_665 ? AL AL Mg1 120.62(5) 3_665 1_665 ? Mg1 AL Mg1 107.94(12) 4_665 1_665 ? AL AL AL 180.0(2) 2_655 2_765 ? AL AL AL 120.0 3_665 2_765 ? Mg1 AL AL 59.38(5) 4_665 2_765 ? Mg1 AL AL 59.38(5) 1_665 2_765 ? AL AL AL 120.0 2_655 3_675 ? AL AL AL 180.00(15) 3_665 3_675 ? Mg1 AL AL 59.38(5) 4_665 3_675 ? Mg1 AL AL 59.38(5) 1_665 3_675 ? AL AL AL 60.0 2_765 3_675 ? AL AL Ca1 64.67(5) 2_655 13_665 ? AL AL Ca1 64.67(5) 3_665 13_665 ? Mg1 AL Ca1 173.58(12) 4_665 13_665 ? Mg1 AL Ca1 65.64(2) 1_665 13_665 ? AL AL Ca1 115.33(5) 2_765 13_665 ? AL AL Ca1 115.33(5) 3_675 13_665 ? AL AL Ca1 64.67(5) 2_655 4_665 ? AL AL Ca1 64.67(5) 3_665 4_665 ? Mg1 AL Ca1 65.64(2) 4_665 4_665 ? Mg1 AL Ca1 173.58(12) 1_665 4_665 ? AL AL Ca1 115.33(5) 2_765 4_665 ? AL AL Ca1 115.33(5) 3_675 4_665 ? Ca1 AL Ca1 120.79(12) 13_665 4_665 ? AL AL Ca1 115.68(6) 2_655 16_656 ? AL AL Ca1 65.03(6) 3_665 16_656 ? Mg1 AL Ca1 65.00(3) 4_665 16_656 ? Mg1 AL Ca1 114.52(7) 1_665 16_656 ? AL AL Ca1 64.32(6) 2_765 16_656 ? AL AL Ca1 114.97(6) 3_675 16_656 ? Ca1 AL Ca1 116.96(6) 13_665 16_656 ? Ca1 AL Ca1 63.44(3) 4_665 16_656 ? AL AL Ca1 115.68(6) 2_655 1_655 ? AL AL Ca1 65.03(6) 3_665 1_655 ? Mg1 AL Ca1 114.52(7) 4_665 1_655 ? Mg1 AL Ca1 65.00(3) 1_665 1_655 ? AL AL Ca1 64.32(6) 2_765 1_655 ? AL AL Ca1 114.97(6) 3_675 1_655 ? Ca1 AL Ca1 63.44(3) 13_665 1_655 ? Ca1 AL Ca1 116.96(6) 4_665 1_655 ? Ca1 AL Ca1 62.37(6) 16_656 1_655 ? AL AL Ca1 65.03(6) 2_655 . ? AL AL Ca1 115.68(6) 3_665 . ? Mg1 AL Ca1 114.52(7) 4_665 . ? Mg1 AL Ca1 65.00(3) 1_665 . ? AL AL Ca1 114.97(6) 2_765 . ? AL AL Ca1 64.32(6) 3_675 . ? Ca1 AL Ca1 63.44(3) 13_665 . ? Ca1 AL Ca1 116.96(6) 4_665 . ? Ca1 AL Ca1 179.26(13) 16_656 . ? Ca1 AL Ca1 117.62(6) 1_655 . ? AL AL Ca1 65.03(6) 2_655 16_556 ? AL AL Ca1 115.68(6) 3_665 16_556 ? Mg1 AL Ca1 65.00(3) 4_665 16_556 ? Mg1 AL Ca1 114.52(7) 1_665 16_556 ? AL AL Ca1 114.97(6) 2_765 16_556 ? AL AL Ca1 64.32(6) 3_675 16_556 ? Ca1 AL Ca1 116.96(6) 13_665 16_556 ? Ca1 AL Ca1 63.44(3) 4_665 16_556 ? Ca1 AL Ca1 117.62(6) 16_656 16_556 ? Ca1 AL Ca1 179.26(13) 1_655 16_556 ? Ca1 AL Ca1 62.37(6) . 16_556 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.671 _refine_diff_density_min -0.890 _refine_diff_density_rms 0.212 #===END CaAl0.93Mg1.07 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'CaAl0.93Mg1.07 _chemical_formula_weight 91.2 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P 63/m m c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 5.935(1) _cell_length_b 5.935(1) _cell_length_c 19.258(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 587.5(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 14.5 _cell_measurement_theta_max 43.4 _exptl_crystal_description irregular shape _exptl_crystal_colour Silver _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.015 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.055 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 2.281 _exptl_absorpt_correction_type numerical (X-shape, stoe & Cie, 1997)) _exptl_absorpt_correction_T_min 0.6717 _exptl_absorpt_correction_T_max 0.7280 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Stoe IPDS (version 2.87) _diffrn_measurement_method f scan _diffrn_detector_area_resol_mean area detector _diffrn_standards_number 6.0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4983 _diffrn_reflns_av_R_equivalents 0.0892 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.96 _diffrn_reflns_theta_max 28.12 _reflns_number_total 318 _reflns_number_gt 191 _reflns_threshold_expression >2sigma(I) _computing_data_collection EXPOSE (Stoe & Cie, 1997) _computing_cell_refinement PIRUM (Werner & Ericsson, 1993) _computing_data_reduction X-RED (Stoe & Cie, 1997) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Atoms (Dowty, 1997) _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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. Unit cell parameters least square refined from 29 measured and indexed lines of a Guinier powder diagram (Cuka, Si (NIST) standard) (program PIRUM (Werner & Ericsson, 1993)) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 318 _refine_ls_number_parameters 18 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0184 _refine_ls_wR_factor_ref 0.0321 _refine_ls_wR_factor_gt 0.0175 _refine_ls_goodness_of_fit_ref 1.881 _refine_ls_restrained_S_all 1.881 _refine_ls_shift/su_max 0.000 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.3333 0.6667 0.34313(5) 0.0116(2) Uani 1 6 d S . . Ca2 Ca 0.0000 0.0000 0.40560(5) 0.0120(3) Uani 1 6 d S . . AL1 Mg 0.3267(3) 0.16336(15) 0.2500 0.0076(3) Uani 1 4 d S . . Al2 Al 0.3333 0.6667 0.62854(7) 0.0149(3) Uani 1 6 d S . . MG1 Al 0.0000 0.5000 0.5000 0.0159(3) Uani 1 4 d S . . 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 Ca1 0.0117(4) 0.0117(4) 0.0113(4) 0.000 0.000 0.0059(2) Ca2 0.0123(4) 0.0123(4) 0.0115(4) 0.000 0.000 0.0061(2) AL1 0.0065(8) 0.0082(6) 0.0076(5) 0.000 0.000 0.0032(4) Al2 0.0155(5) 0.0155(5) 0.0137(5) 0.000 0.000 0.0078(3) MG1 0.0145(9) 0.0161(6) 0.0165(6) -0.0001(2) -0.0001(5) 0.0073(4) _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 Ca1 AL1 3.4737(6) 2 ? Ca1 AL1 3.4737(6) 3_565 ? Ca1 AL1 3.4737(6) 1_565 ? Ca1 AL1 3.4737(6) 2_665 ? Ca1 AL1 3.4737(6) . ? Ca1 AL1 3.4737(7) 3_665 ? Ca1 Al2 3.4751(6) 13_676 ? Ca1 Al2 3.4751(6) 13_566 ? Ca1 Al2 3.4751(6) 13_666 ? Ca1 MG1 3.4809(10) 3_565 ? Ca1 MG1 3.4809(10) . ? Ca1 MG1 3.4809(10) 2_665 ? Ca2 AL1 3.4427(13) 3 ? Ca2 AL1 3.4427(13) 2 ? Ca2 AL1 3.4427(13) . ? Ca2 MG1 3.4864(7) 2_665 ? Ca2 MG1 3.4864(7) 3 ? Ca2 MG1 3.4864(7) . ? Ca2 MG1 3.4864(7) 2 ? Ca2 MG1 3.4864(7) 3_455 ? Ca2 MG1 3.4864(7) 1_545 ? Ca2 Al2 3.4945(6) 13_566 ? Ca2 Al2 3.4945(6) 13_556 ? Ca2 Al2 3.4945(6) 13_666 ? AL1 AL1 2.913(3) 3 ? AL1 AL1 2.913(3) 2 ? AL1 Al2 2.9258(15) 13_666 ? AL1 Al2 2.9258(15) 4_664 ? AL1 AL1 3.031(3) 3_665 ? AL1 AL1 3.031(3) 2_655 ? AL1 Ca2 3.4427(13) 16_556 ? AL1 Ca1 3.4737(6) 16_546 ? AL1 Ca1 3.4737(6) 1_545 ? AL1 Ca1 3.4737(7) 16_556 ? Al2 AL1 2.9258(15) 14_566 ? Al2 AL1 2.9258(15) 13_666 ? Al2 AL1 2.9258(15) 15_556 ? Al2 Ca1 3.4751(6) 13_676 ? Al2 Ca1 3.4751(6) 13_566 ? Al2 Ca1 3.4751(6) 13_666 ? Al2 Ca2 3.4945(6) 13_566 ? Al2 Ca2 3.4945(6) 13_556 ? Al2 Ca2 3.4945(6) 13_666 ? MG1 MG1 2.9721(4) 3_565 ? MG1 MG1 2.9721(4) 3_455 ? MG1 MG1 2.9721(5) 2_665 ? MG1 MG1 2.9721(4) 2_565 ? MG1 Ca1 3.4809(10) 13_566 ? MG1 Ca2 3.4864(7) 13_566 ? MG1 Ca2 3.4864(7) 13_556 ? MG1 Ca2 3.4864(7) 1_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 AL1 Ca1 AL1 51.73(5) 2 3_565 ? AL1 Ca1 AL1 95.63(2) 2 1_565 ? AL1 Ca1 AL1 49.58(5) 3_565 1_565 ? AL1 Ca1 AL1 117.65(3) 2 2_665 ? AL1 Ca1 AL1 95.63(2) 3_565 2_665 ? AL1 Ca1 AL1 51.73(5) 1_565 2_665 ? AL1 Ca1 AL1 49.58(5) 2 . ? AL1 Ca1 AL1 95.63(2) 3_565 . ? AL1 Ca1 AL1 117.65(3) 1_565 . ? AL1 Ca1 AL1 95.63(2) 2_665 . ? AL1 Ca1 AL1 95.63(2) 2 3_665 ? AL1 Ca1 AL1 117.65(3) 3_565 3_665 ? AL1 Ca1 AL1 95.63(2) 1_565 3_665 ? AL1 Ca1 AL1 49.58(5) 2_665 3_665 ? AL1 Ca1 AL1 51.73(5) . 3_665 ? AL1 Ca1 Al2 144.89(3) 2 13_676 ? AL1 Ca1 Al2 94.12(3) 3_565 13_676 ? AL1 Ca1 Al2 49.80(3) 1_565 13_676 ? AL1 Ca1 Al2 49.80(3) 2_665 13_676 ? AL1 Ca1 Al2 144.89(3) . 13_676 ? AL1 Ca1 Al2 94.12(3) 3_665 13_676 ? AL1 Ca1 Al2 49.80(3) 2 13_566 ? AL1 Ca1 Al2 49.80(3) 3_565 13_566 ? AL1 Ca1 Al2 94.12(3) 1_565 13_566 ? AL1 Ca1 Al2 144.89(3) 2_665 13_566 ? AL1 Ca1 Al2 94.12(3) . 13_566 ? AL1 Ca1 Al2 144.89(3) 3_665 13_566 ? Al2 Ca1 Al2 117.571(15) 13_676 13_566 ? AL1 Ca1 Al2 94.12(3) 2 13_666 ? AL1 Ca1 Al2 144.89(3) 3_565 13_666 ? AL1 Ca1 Al2 144.89(3) 1_565 13_666 ? AL1 Ca1 Al2 94.12(3) 2_665 13_666 ? AL1 Ca1 Al2 49.80(3) . 13_666 ? AL1 Ca1 Al2 49.80(3) 3_665 13_666 ? Al2 Ca1 Al2 117.571(16) 13_676 13_666 ? Al2 Ca1 Al2 117.571(16) 13_566 13_666 ? AL1 Ca1 MG1 144.88(2) 2 3_565 ? AL1 Ca1 MG1 116.454(18) 3_565 3_565 ? AL1 Ca1 MG1 95.019(15) 1_565 3_565 ? AL1 Ca1 MG1 95.019(15) 2_665 3_565 ? AL1 Ca1 MG1 144.88(2) . 3_565 ? AL1 Ca1 MG1 116.454(19) 3_665 3_565 ? Al2 Ca1 MG1 51.41(3) 13_676 3_565 ? Al2 Ca1 MG1 96.11(3) 13_566 3_565 ? Al2 Ca1 MG1 96.11(3) 13_666 3_565 ? AL1 Ca1 MG1 95.019(15) 2 . ? AL1 Ca1 MG1 95.019(15) 3_565 . ? AL1 Ca1 MG1 116.454(19) 1_565 . ? AL1 Ca1 MG1 144.88(2) 2_665 . ? AL1 Ca1 MG1 116.454(19) . . ? AL1 Ca1 MG1 144.88(2) 3_665 . ? Al2 Ca1 MG1 96.11(3) 13_676 . ? Al2 Ca1 MG1 51.41(2) 13_566 . ? Al2 Ca1 MG1 96.11(3) 13_666 . ? MG1 Ca1 MG1 50.543(17) 3_565 . ? AL1 Ca1 MG1 116.454(18) 2 2_665 ? AL1 Ca1 MG1 144.88(2) 3_565 2_665 ? AL1 Ca1 MG1 144.88(2) 1_565 2_665 ? AL1 Ca1 MG1 116.454(19) 2_665 2_665 ? AL1 Ca1 MG1 95.019(15) . 2_665 ? AL1 Ca1 MG1 95.019(15) 3_665 2_665 ? Al2 Ca1 MG1 96.11(3) 13_676 2_665 ? Al2 Ca1 MG1 96.11(3) 13_566 2_665 ? Al2 Ca1 MG1 51.41(2) 13_666 2_665 ? MG1 Ca1 MG1 50.543(17) 3_565 2_665 ? MG1 Ca1 MG1 50.543(17) . 2_665 ? AL1 Ca2 AL1 50.06(4) 3 2 ? AL1 Ca2 AL1 50.06(4) 3 . ? AL1 Ca2 AL1 50.06(4) 2 . ? AL1 Ca2 MG1 144.77(2) 3 2_665 ? AL1 Ca2 MG1 117.138(14) 2 2_665 ? AL1 Ca2 MG1 95.48(3) . 2_665 ? AL1 Ca2 MG1 117.138(14) 3 3 ? AL1 Ca2 MG1 144.77(2) 2 3 ? AL1 Ca2 MG1 95.48(2) . 3 ? MG1 Ca2 MG1 50.458(9) 2_665 3 ? AL1 Ca2 MG1 144.77(2) 3 . ? AL1 Ca2 MG1 95.48(3) 2 . ? AL1 Ca2 MG1 117.138(14) . . ? MG1 Ca2 MG1 50.458(9) 2_665 . ? MG1 Ca2 MG1 95.17(2) 3 . ? AL1 Ca2 MG1 95.48(3) 3 2 ? AL1 Ca2 MG1 117.138(14) 2 2 ? AL1 Ca2 MG1 144.77(2) . 2 ? MG1 Ca2 MG1 116.96(3) 2_665 2 ? MG1 Ca2 MG1 95.17(2) 3 2 ? MG1 Ca2 MG1 95.17(2) . 2 ? AL1 Ca2 MG1 117.138(14) 3 3_455 ? AL1 Ca2 MG1 95.48(3) 2 3_455 ? AL1 Ca2 MG1 144.77(2) . 3_455 ? MG1 Ca2 MG1 95.17(2) 2_665 3_455 ? MG1 Ca2 MG1 116.96(3) 3 3_455 ? MG1 Ca2 MG1 50.458(9) . 3_455 ? MG1 Ca2 MG1 50.458(9) 2 3_455 ? AL1 Ca2 MG1 95.48(2) 3 1_545 ? AL1 Ca2 MG1 144.77(2) 2 1_545 ? AL1 Ca2 MG1 117.138(14) . 1_545 ? MG1 Ca2 MG1 95.17(2) 2_665 1_545 ? MG1 Ca2 MG1 50.458(9) 3 1_545 ? MG1 Ca2 MG1 116.96(3) . 1_545 ? MG1 Ca2 MG1 50.458(9) 2 1_545 ? MG1 Ca2 MG1 95.17(2) 3_455 1_545 ? AL1 Ca2 Al2 94.32(3) 3 13_566 ? AL1 Ca2 Al2 49.88(3) 2 13_566 ? AL1 Ca2 Al2 94.32(3) . 13_566 ? MG1 Ca2 Al2 95.658(15) 2_665 13_566 ? MG1 Ca2 Al2 145.45(3) 3 13_566 ? MG1 Ca2 Al2 51.21(2) . 13_566 ? MG1 Ca2 Al2 95.658(15) 2 13_566 ? MG1 Ca2 Al2 51.21(2) 3_455 13_566 ? MG1 Ca2 Al2 145.45(3) 1_545 13_566 ? AL1 Ca2 Al2 49.88(3) 3 13_556 ? AL1 Ca2 Al2 94.32(3) 2 13_556 ? AL1 Ca2 Al2 94.32(3) . 13_556 ? MG1 Ca2 Al2 145.45(3) 2_665 13_556 ? MG1 Ca2 Al2 95.658(14) 3 13_556 ? MG1 Ca2 Al2 145.45(3) . 13_556 ? MG1 Ca2 Al2 51.21(2) 2 13_556 ? MG1 Ca2 Al2 95.658(15) 3_455 13_556 ? MG1 Ca2 Al2 51.21(2) 1_545 13_556 ? Al2 Ca2 Al2 116.528(19) 13_566 13_556 ? AL1 Ca2 Al2 94.32(3) 3 13_666 ? AL1 Ca2 Al2 94.32(3) 2 13_666 ? AL1 Ca2 Al2 49.88(3) . 13_666 ? MG1 Ca2 Al2 51.21(2) 2_665 13_666 ? MG1 Ca2 Al2 51.21(2) 3 13_666 ? MG1 Ca2 Al2 95.658(15) . 13_666 ? MG1 Ca2 Al2 145.45(3) 2 13_666 ? MG1 Ca2 Al2 145.45(3) 3_455 13_666 ? MG1 Ca2 Al2 95.658(15) 1_545 13_666 ? Al2 Ca2 Al2 116.528(19) 13_566 13_666 ? Al2 Ca2 Al2 116.528(19) 13_556 13_666 ? AL1 AL1 AL1 60.0 3 2 ? AL1 AL1 Al2 121.20(2) 3 13_666 ? AL1 AL1 Al2 121.20(2) 2 13_666 ? AL1 AL1 Al2 121.20(2) 3 4_664 ? AL1 AL1 Al2 121.20(2) 2 4_664 ? Al2 AL1 Al2 106.53(6) 13_666 4_664 ? AL1 AL1 AL1 180.0 3 3_665 ? AL1 AL1 AL1 120.0 2 3_665 ? Al2 AL1 AL1 58.80(2) 13_666 3_665 ? Al2 AL1 AL1 58.80(2) 4_664 3_665 ? AL1 AL1 AL1 120.0 3 2_655 ? AL1 AL1 AL1 180.00(6) 2 2_655 ? Al2 AL1 AL1 58.80(2) 13_666 2_655 ? Al2 AL1 AL1 58.80(2) 4_664 2_655 ? AL1 AL1 AL1 60.0 3_665 2_655 ? AL1 AL1 Ca2 64.97(2) 3 16_556 ? AL1 AL1 Ca2 64.97(2) 2 16_556 ? Al2 AL1 Ca2 172.51(5) 13_666 16_556 ? Al2 AL1 Ca2 65.98(2) 4_664 16_556 ? AL1 AL1 Ca2 115.03(2) 3_665 16_556 ? AL1 AL1 Ca2 115.03(2) 2_655 16_556 ? AL1 AL1 Ca2 64.97(2) 3 . ? AL1 AL1 Ca2 64.97(2) 2 . ? Al2 AL1 Ca2 65.98(2) 13_666 . ? Al2 AL1 Ca2 172.51(5) 4_664 . ? AL1 AL1 Ca2 115.03(2) 3_665 . ? AL1 AL1 Ca2 115.03(2) 2_655 . ? Ca2 AL1 Ca2 121.51(5) 16_556 . ? AL1 AL1 Ca1 65.21(2) 3 16_546 ? AL1 AL1 Ca1 115.87(2) 2 16_546 ? Al2 AL1 Ca1 114.14(3) 13_666 16_546 ? Al2 AL1 Ca1 65.124(15) 4_664 16_546 ? AL1 AL1 Ca1 114.79(2) 3_665 16_546 ? AL1 AL1 Ca1 64.13(2) 2_655 16_546 ? Ca2 AL1 Ca1 63.460(16) 16_556 16_546 ? Ca2 AL1 Ca1 117.15(2) . 16_546 ? AL1 AL1 Ca1 65.21(2) 3 1_545 ? AL1 AL1 Ca1 115.87(2) 2 1_545 ? Al2 AL1 Ca1 65.124(15) 13_666 1_545 ? Al2 AL1 Ca1 114.14(3) 4_664 1_545 ? AL1 AL1 Ca1 114.79(2) 3_665 1_545 ? AL1 AL1 Ca1 64.13(2) 2_655 1_545 ? Ca2 AL1 Ca1 117.15(2) 16_556 1_545 ? Ca2 AL1 Ca1 63.460(16) . 1_545 ? Ca1 AL1 Ca1 62.34(3) 16_546 1_545 ? AL1 AL1 Ca1 115.87(2) 3 . ? AL1 AL1 Ca1 65.21(2) 2 . ? Al2 AL1 Ca1 65.124(15) 13_666 . ? Al2 AL1 Ca1 114.14(3) 4_664 . ? AL1 AL1 Ca1 64.13(2) 3_665 . ? AL1 AL1 Ca1 114.79(2) 2_655 . ? Ca2 AL1 Ca1 117.15(2) 16_556 . ? Ca2 AL1 Ca1 63.460(16) . . ? Ca1 AL1 Ca1 178.88(5) 16_546 . ? Ca1 AL1 Ca1 117.65(3) 1_545 . ? AL1 AL1 Ca1 115.87(2) 3 16_556 ? AL1 AL1 Ca1 65.21(2) 2 16_556 ? Al2 AL1 Ca1 114.14(3) 13_666 16_556 ? Al2 AL1 Ca1 65.124(15) 4_664 16_556 ? AL1 AL1 Ca1 64.13(2) 3_665 16_556 ? AL1 AL1 Ca1 114.79(2) 2_655 16_556 ? Ca2 AL1 Ca1 63.460(16) 16_556 16_556 ? Ca2 AL1 Ca1 117.15(2) . 16_556 ? Ca1 AL1 Ca1 117.65(3) 16_546 16_556 ? Ca1 AL1 Ca1 178.88(5) 1_545 16_556 ? Ca1 AL1 Ca1 62.34(3) . 16_556 ? AL1 Al2 AL1 62.39(5) 14_566 13_666 ? AL1 Al2 AL1 62.39(5) 14_566 15_556 ? AL1 Al2 AL1 62.39(5) 13_666 15_556 ? AL1 Al2 Ca1 65.07(2) 14_566 13_676 ? AL1 Al2 Ca1 65.07(2) 13_666 13_676 ? AL1 Al2 Ca1 117.68(5) 15_556 13_676 ? AL1 Al2 Ca1 65.07(2) 14_566 13_566 ? AL1 Al2 Ca1 117.68(5) 13_666 13_566 ? AL1 Al2 Ca1 65.07(2) 15_556 13_566 ? Ca1 Al2 Ca1 117.571(15) 13_676 13_566 ? AL1 Al2 Ca1 117.68(5) 14_566 13_666 ? AL1 Al2 Ca1 65.07(2) 13_666 13_666 ? AL1 Al2 Ca1 65.07(2) 15_556 13_666 ? Ca1 Al2 Ca1 117.571(16) 13_676 13_666 ? Ca1 Al2 Ca1 117.571(16) 13_566 13_666 ? AL1 Al2 Ca2 64.14(3) 14_566 13_566 ? AL1 Al2 Ca2 116.41(3) 13_666 13_566 ? AL1 Al2 Ca2 116.41(3) 15_556 13_566 ? Ca1 Al2 Ca2 62.921(5) 13_676 13_566 ? Ca1 Al2 Ca2 62.921(5) 13_566 13_566 ? Ca1 Al2 Ca2 178.18(6) 13_666 13_566 ? AL1 Al2 Ca2 116.41(3) 14_566 13_556 ? AL1 Al2 Ca2 116.41(3) 13_666 13_556 ? AL1 Al2 Ca2 64.14(3) 15_556 13_556 ? Ca1 Al2 Ca2 178.18(6) 13_676 13_556 ? Ca1 Al2 Ca2 62.921(5) 13_566 13_556 ? Ca1 Al2 Ca2 62.921(5) 13_666 13_556 ? Ca2 Al2 Ca2 116.528(19) 13_566 13_556 ? AL1 Al2 Ca2 116.41(3) 14_566 13_666 ? AL1 Al2 Ca2 64.14(3) 13_666 13_666 ? AL1 Al2 Ca2 116.41(3) 15_556 13_666 ? Ca1 Al2 Ca2 62.921(5) 13_676 13_666 ? Ca1 Al2 Ca2 178.18(6) 13_566 13_666 ? Ca1 Al2 Ca2 62.921(5) 13_666 13_666 ? Ca2 Al2 Ca2 116.528(19) 13_566 13_666 ? Ca2 Al2 Ca2 116.528(19) 13_556 13_666 ? MG1 MG1 MG1 180.0 3_565 3_455 ? MG1 MG1 MG1 60.0 3_565 2_665 ? MG1 MG1 MG1 120.0 3_455 2_665 ? MG1 MG1 MG1 120.0 3_565 2_565 ? MG1 MG1 MG1 60.0 3_455 2_565 ? MG1 MG1 MG1 180.0 2_665 2_565 ? MG1 MG1 Ca1 64.729(8) 3_565 . ? MG1 MG1 Ca1 115.271(8) 3_455 . ? MG1 MG1 Ca1 64.729(8) 2_665 . ? MG1 MG1 Ca1 115.271(8) 2_565 . ? MG1 MG1 Ca1 115.271(8) 3_565 13_566 ? MG1 MG1 Ca1 64.729(8) 3_455 13_566 ? MG1 MG1 Ca1 115.271(8) 2_665 13_566 ? MG1 MG1 Ca1 64.729(8) 2_565 13_566 ? Ca1 MG1 Ca1 180.0 . 13_566 ? MG1 MG1 Ca2 64.771(4) 3_565 13_566 ? MG1 MG1 Ca2 115.229(4) 3_455 13_566 ? MG1 MG1 Ca2 115.229(4) 2_665 13_566 ? MG1 MG1 Ca2 64.771(4) 2_565 13_566 ? Ca1 MG1 Ca2 117.055(14) . 13_566 ? Ca1 MG1 Ca2 62.945(14) 13_566 13_566 ? MG1 MG1 Ca2 115.229(4) 3_565 . ? MG1 MG1 Ca2 64.771(4) 3_455 . ? MG1 MG1 Ca2 64.771(4) 2_665 . ? MG1 MG1 Ca2 115.229(4) 2_565 . ? Ca1 MG1 Ca2 62.945(14) . . ? Ca1 MG1 Ca2 117.055(14) 13_566 . ? Ca2 MG1 Ca2 180.0 13_566 . ? MG1 MG1 Ca2 115.229(4) 3_565 13_556 ? MG1 MG1 Ca2 64.771(4) 3_455 13_556 ? MG1 MG1 Ca2 64.771(4) 2_665 13_556 ? MG1 MG1 Ca2 115.229(4) 2_565 13_556 ? Ca1 MG1 Ca2 117.055(14) . 13_556 ? Ca1 MG1 Ca2 62.945(14) 13_566 13_556 ? Ca2 MG1 Ca2 116.96(3) 13_566 13_556 ? Ca2 MG1 Ca2 63.04(3) . 13_556 ? MG1 MG1 Ca2 64.771(4) 3_565 1_565 ? MG1 MG1 Ca2 115.229(4) 3_455 1_565 ? MG1 MG1 Ca2 115.229(4) 2_665 1_565 ? MG1 MG1 Ca2 64.771(4) 2_565 1_565 ? Ca1 MG1 Ca2 62.945(14) . 1_565 ? Ca1 MG1 Ca2 117.055(14) 13_566 1_565 ? Ca2 MG1 Ca2 63.04(3) 13_566 1_565 ? Ca2 MG1 Ca2 116.96(3) . 1_565 ? Ca2 MG1 Ca2 180.0 13_556 1_565 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.12 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.427 _refine_diff_density_min -1.341 _refine_diff_density_rms 0.245 #===END CaAl1.34Mg0.66 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum CaAl1.34Mg0.66 _chemical_formula_weight 92.3 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P 63/m m c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 5.8353(4) _cell_length_b 5.8353(4) _cell_length_c 18.897(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 557.25(10) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 14.7 _cell_measurement_theta_max 38.4 _exptl_crystal_description irregular shape _exptl_crystal_colour silver _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 362 _exptl_absorpt_coefficient_mu 2.441 _exptl_absorpt_correction_type numerical (X-shape, stoe & Cie, 1997)) _exptl_absorpt_correction_T_min 0.5692 _exptl_absorpt_correction_T_max 0.7675 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ?Stoe IPDS (version 2.87) _diffrn_measurement_method f scan _diffrn_detector_area_resol_mean area detector _diffrn_standards_number 6.0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4519 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.03 _diffrn_reflns_theta_max 28.09 _reflns_number_total 305 _reflns_number_gt 168 _reflns_threshold_expression >2sigma(I) _computing_data_collection EXPOSE (Stoe & Cie, 1997) _computing_cell_refinement PIRUM (Werner & Ericsson, 1993) _computing_data_reduction X-RED (Stoe & Cie, 1997) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Atoms (Dowty, 1997) _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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. Unit cell parameters least square refined from 20 measured and indexed lines of a Guinier powder diagram (Cuka, Si (NIST) standard) (program PIRUM (Werner & Ericsson, 1993)) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0161P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 305 _refine_ls_number_parameters 10 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0409 _refine_ls_wR_factor_gt 0.0352 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.000 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.3333 0.6667 0.34300(6) 0.0107(2) Uiso 1 6 d S . . Ca2 Ca 0.0000 0.0000 0.40594(6) 0.0116(3) Uiso 1 6 d S . . AL1 Mg 0.3260(3) 0.16302(17) 0.2500 0.0056(3) Uiso 1 4 d S . . AL2 Mg 0.3333 0.6667 0.62939(9) 0.0066(3) Uiso 1 6 d S . . Mg1 Mg 0.0000 0.5000 0.5000 0.0076(3) Uiso 1 4 d S . . _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 Ca1 AL1 3.4062(6) 2 ? Ca1 AL1 3.4062(6) 1_565 ? Ca1 AL1 3.4062(6) 3_565 ? Ca1 AL1 3.4062(6) 3_665 ? Ca1 AL1 3.4062(6) 2_665 ? Ca1 AL1 3.4062(6) . ? Ca1 AL2 3.4092(4) 13_676 ? Ca1 AL2 3.4092(4) 13_566 ? Ca1 AL2 3.4092(4) 13_666 ? Ca1 Mg1 3.4117(10) 3_565 ? Ca1 Mg1 3.4117(10) . ? Ca1 Mg1 3.4117(10) 2_665 ? Ca2 AL1 3.3762(13) 3 ? Ca2 AL1 3.3762(13) 2 ? Ca2 AL1 3.3762(13) . ? Ca2 Mg1 3.4164(6) 2_665 ? Ca2 Mg1 3.4164(6) 3 ? Ca2 Mg1 3.4164(6) . ? Ca2 Mg1 3.4164(6) 2 ? Ca2 Mg1 3.4164(6) 3_455 ? Ca2 Mg1 3.4164(6) 1_545 ? Ca2 AL2 3.4345(5) 13_566 ? Ca2 AL2 3.4345(5) 13_556 ? Ca2 AL2 3.4345(5) 13_666 ? AL1 AL1 2.854(3) 3 ? AL1 AL1 2.854(3) 2 ? AL1 AL2 2.8562(17) 13_666 ? AL1 AL2 2.8562(17) 4_664 ? AL1 AL1 2.981(3) 3_665 ? AL1 AL1 2.981(3) 2_655 ? AL1 Ca2 3.3762(13) 16_556 ? AL1 Ca1 3.4062(6) 16_546 ? AL1 Ca1 3.4062(6) 1_545 ? AL1 Ca1 3.4062(6) 16_556 ? AL2 AL1 2.8562(17) 14_566 ? AL2 AL1 2.8562(17) 13_666 ? AL2 AL1 2.8562(17) 15_556 ? AL2 Mg1 2.9691(14) . ? AL2 Mg1 2.9691(14) 3_565 ? AL2 Mg1 2.9691(14) 2_665 ? AL2 Ca1 3.4092(4) 13_676 ? AL2 Ca1 3.4092(4) 13_566 ? AL2 Ca1 3.4092(4) 13_666 ? AL2 Ca2 3.4345(5) 13_566 ? AL2 Ca2 3.4345(5) 13_556 ? AL2 Ca2 3.4345(5) 13_666 ? Mg1 Mg1 2.9177(2) 3_565 ? Mg1 Mg1 2.9177(2) 3_455 ? Mg1 Mg1 2.9177(2) 2_665 ? Mg1 Mg1 2.9177(2) 2_565 ? Mg1 AL2 2.9691(14) 13_566 ? Mg1 Ca1 3.4117(10) 13_566 ? Mg1 Ca2 3.4164(6) 13_566 ? Mg1 Ca2 3.4164(6) 1_565 ? Mg1 Ca2 3.4164(6) 13_556 ? 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 AL1 Ca1 AL1 95.78(2) 2 1_565 ? AL1 Ca1 AL1 51.91(5) 2 3_565 ? AL1 Ca1 AL1 49.53(6) 1_565 3_565 ? AL1 Ca1 AL1 95.78(2) 2 3_665 ? AL1 Ca1 AL1 95.78(2) 1_565 3_665 ? AL1 Ca1 AL1 117.87(3) 3_565 3_665 ? AL1 Ca1 AL1 117.87(3) 2 2_665 ? AL1 Ca1 AL1 51.91(6) 1_565 2_665 ? AL1 Ca1 AL1 95.78(2) 3_565 2_665 ? AL1 Ca1 AL1 49.53(6) 3_665 2_665 ? AL1 Ca1 AL1 49.53(5) 2 . ? AL1 Ca1 AL1 117.87(3) 1_565 . ? AL1 Ca1 AL1 95.78(2) 3_565 . ? AL1 Ca1 AL1 51.91(5) 3_665 . ? AL1 Ca1 AL1 95.78(2) 2_665 . ? AL1 Ca1 AL2 144.82(4) 2 13_676 ? AL1 Ca1 AL2 49.55(3) 1_565 13_676 ? AL1 Ca1 AL2 93.92(3) 3_565 13_676 ? AL1 Ca1 AL2 93.92(3) 3_665 13_676 ? AL1 Ca1 AL2 49.55(3) 2_665 13_676 ? AL1 Ca1 AL2 144.82(4) . 13_676 ? AL1 Ca1 AL2 49.55(3) 2 13_566 ? AL1 Ca1 AL2 93.92(3) 1_565 13_566 ? AL1 Ca1 AL2 49.55(3) 3_565 13_566 ? AL1 Ca1 AL2 144.82(4) 3_665 13_566 ? AL1 Ca1 AL2 144.82(4) 2_665 13_566 ? AL1 Ca1 AL2 93.92(3) . 13_566 ? AL2 Ca1 AL2 117.701(19) 13_676 13_566 ? AL1 Ca1 AL2 93.92(3) 2 13_666 ? AL1 Ca1 AL2 144.82(4) 1_565 13_666 ? AL1 Ca1 AL2 144.82(4) 3_565 13_666 ? AL1 Ca1 AL2 49.55(3) 3_665 13_666 ? AL1 Ca1 AL2 93.92(3) 2_665 13_666 ? AL1 Ca1 AL2 49.55(3) . 13_666 ? AL2 Ca1 AL2 117.701(19) 13_676 13_666 ? AL2 Ca1 AL2 117.701(19) 13_566 13_666 ? AL1 Ca1 Mg1 144.84(2) 2 3_565 ? AL1 Ca1 Mg1 94.880(12) 1_565 3_565 ? AL1 Ca1 Mg1 116.316(19) 3_565 3_565 ? AL1 Ca1 Mg1 116.32(2) 3_665 3_565 ? AL1 Ca1 Mg1 94.880(12) 2_665 3_565 ? AL1 Ca1 Mg1 144.84(2) . 3_565 ? AL2 Ca1 Mg1 51.61(3) 13_676 3_565 ? AL2 Ca1 Mg1 96.36(4) 13_566 3_565 ? AL2 Ca1 Mg1 96.36(4) 13_666 3_565 ? AL1 Ca1 Mg1 94.880(12) 2 . ? AL1 Ca1 Mg1 116.32(2) 1_565 . ? AL1 Ca1 Mg1 94.880(12) 3_565 . ? AL1 Ca1 Mg1 144.84(2) 3_665 . ? AL1 Ca1 Mg1 144.84(2) 2_665 . ? AL1 Ca1 Mg1 116.32(2) . . ? AL2 Ca1 Mg1 96.36(4) 13_676 . ? AL2 Ca1 Mg1 51.61(3) 13_566 . ? AL2 Ca1 Mg1 96.36(4) 13_666 . ? Mg1 Ca1 Mg1 50.630(17) 3_565 . ? AL1 Ca1 Mg1 116.316(19) 2 2_665 ? AL1 Ca1 Mg1 144.84(2) 1_565 2_665 ? AL1 Ca1 Mg1 144.84(2) 3_565 2_665 ? AL1 Ca1 Mg1 94.880(12) 3_665 2_665 ? AL1 Ca1 Mg1 116.316(19) 2_665 2_665 ? AL1 Ca1 Mg1 94.880(12) . 2_665 ? AL2 Ca1 Mg1 96.36(4) 13_676 2_665 ? AL2 Ca1 Mg1 96.36(4) 13_566 2_665 ? AL2 Ca1 Mg1 51.61(3) 13_666 2_665 ? Mg1 Ca1 Mg1 50.630(17) 3_565 2_665 ? Mg1 Ca1 Mg1 50.630(17) . 2_665 ? AL1 Ca2 AL1 50.00(5) 3 2 ? AL1 Ca2 AL1 50.00(5) 3 . ? AL1 Ca2 AL1 50.00(5) 2 . ? AL1 Ca2 Mg1 144.59(3) 3 2_665 ? AL1 Ca2 Mg1 117.006(13) 2 2_665 ? AL1 Ca2 Mg1 95.34(2) . 2_665 ? AL1 Ca2 Mg1 117.006(14) 3 3 ? AL1 Ca2 Mg1 144.59(3) 2 3 ? AL1 Ca2 Mg1 95.34(2) . 3 ? Mg1 Ca2 Mg1 50.555(10) 2_665 3 ? AL1 Ca2 Mg1 144.59(3) 3 . ? AL1 Ca2 Mg1 95.34(2) 2 . ? AL1 Ca2 Mg1 117.006(13) . . ? Mg1 Ca2 Mg1 50.555(10) 2_665 . ? Mg1 Ca2 Mg1 95.39(2) 3 . ? AL1 Ca2 Mg1 95.34(2) 3 2 ? AL1 Ca2 Mg1 117.006(14) 2 2 ? AL1 Ca2 Mg1 144.59(3) . 2 ? Mg1 Ca2 Mg1 117.30(3) 2_665 2 ? Mg1 Ca2 Mg1 95.39(2) 3 2 ? Mg1 Ca2 Mg1 95.39(2) . 2 ? AL1 Ca2 Mg1 117.006(13) 3 3_455 ? AL1 Ca2 Mg1 95.34(2) 2 3_455 ? AL1 Ca2 Mg1 144.59(3) . 3_455 ? Mg1 Ca2 Mg1 95.39(2) 2_665 3_455 ? Mg1 Ca2 Mg1 117.30(3) 3 3_455 ? Mg1 Ca2 Mg1 50.555(10) . 3_455 ? Mg1 Ca2 Mg1 50.555(10) 2 3_455 ? AL1 Ca2 Mg1 95.34(2) 3 1_545 ? AL1 Ca2 Mg1 144.59(3) 2 1_545 ? AL1 Ca2 Mg1 117.006(13) . 1_545 ? Mg1 Ca2 Mg1 95.39(2) 2_665 1_545 ? Mg1 Ca2 Mg1 50.555(10) 3 1_545 ? Mg1 Ca2 Mg1 117.30(3) . 1_545 ? Mg1 Ca2 Mg1 50.555(10) 2 1_545 ? Mg1 Ca2 Mg1 95.39(2) 3_455 1_545 ? AL1 Ca2 AL2 94.00(4) 3 13_566 ? AL1 Ca2 AL2 49.58(4) 2 13_566 ? AL1 Ca2 AL2 94.00(4) . 13_566 ? Mg1 Ca2 AL2 95.804(18) 2_665 13_566 ? Mg1 Ca2 AL2 145.75(3) 3 13_566 ? Mg1 Ca2 AL2 51.36(2) . 13_566 ? Mg1 Ca2 AL2 95.804(18) 2 13_566 ? Mg1 Ca2 AL2 51.36(2) 3_455 13_566 ? Mg1 Ca2 AL2 145.75(3) 1_545 13_566 ? AL1 Ca2 AL2 49.58(4) 3 13_556 ? AL1 Ca2 AL2 94.00(4) 2 13_556 ? AL1 Ca2 AL2 94.00(4) . 13_556 ? Mg1 Ca2 AL2 145.75(3) 2_665 13_556 ? Mg1 Ca2 AL2 95.804(18) 3 13_556 ? Mg1 Ca2 AL2 145.75(3) . 13_556 ? Mg1 Ca2 AL2 51.36(2) 2 13_556 ? Mg1 Ca2 AL2 95.804(18) 3_455 13_556 ? Mg1 Ca2 AL2 51.36(2) 1_545 13_556 ? AL2 Ca2 AL2 116.32(2) 13_566 13_556 ? AL1 Ca2 AL2 94.00(4) 3 13_666 ? AL1 Ca2 AL2 94.00(4) 2 13_666 ? AL1 Ca2 AL2 49.58(4) . 13_666 ? Mg1 Ca2 AL2 51.36(2) 2_665 13_666 ? Mg1 Ca2 AL2 51.36(2) 3 13_666 ? Mg1 Ca2 AL2 95.804(18) . 13_666 ? Mg1 Ca2 AL2 145.75(3) 2 13_666 ? Mg1 Ca2 AL2 145.75(3) 3_455 13_666 ? Mg1 Ca2 AL2 95.804(18) 1_545 13_666 ? AL2 Ca2 AL2 116.32(2) 13_566 13_666 ? AL2 Ca2 AL2 116.32(2) 13_556 13_666 ? AL1 AL1 AL1 60.0 3 2 ? AL1 AL1 AL2 121.46(3) 3 13_666 ? AL1 AL1 AL2 121.46(3) 2 13_666 ? AL1 AL1 AL2 121.46(3) 3 4_664 ? AL1 AL1 AL2 121.46(3) 2 4_664 ? AL2 AL1 AL2 105.88(7) 13_666 4_664 ? AL1 AL1 AL1 180.00(10) 3 3_665 ? AL1 AL1 AL1 120.0 2 3_665 ? AL2 AL1 AL1 58.54(3) 13_666 3_665 ? AL2 AL1 AL1 58.54(3) 4_664 3_665 ? AL1 AL1 AL1 120.0 3 2_655 ? AL1 AL1 AL1 180.00(7) 2 2_655 ? AL2 AL1 AL1 58.54(3) 13_666 2_655 ? AL2 AL1 AL1 58.54(3) 4_664 2_655 ? AL1 AL1 AL1 60.0 3_665 2_655 ? AL1 AL1 Ca2 65.00(2) 3 16_556 ? AL1 AL1 Ca2 65.00(2) 2 16_556 ? AL2 AL1 Ca2 172.15(6) 13_666 16_556 ? AL2 AL1 Ca2 66.27(2) 4_664 16_556 ? AL1 AL1 Ca2 115.00(2) 3_665 16_556 ? AL1 AL1 Ca2 115.00(2) 2_655 16_556 ? AL1 AL1 Ca2 65.00(2) 3 . ? AL1 AL1 Ca2 65.00(2) 2 . ? AL2 AL1 Ca2 66.27(2) 13_666 . ? AL2 AL1 Ca2 172.15(6) 4_664 . ? AL1 AL1 Ca2 115.00(2) 3_665 . ? AL1 AL1 Ca2 115.00(2) 2_655 . ? Ca2 AL1 Ca2 121.58(5) 16_556 . ? AL1 AL1 Ca1 65.23(3) 3 16_546 ? AL1 AL1 Ca1 115.95(3) 2 16_546 ? AL2 AL1 Ca1 113.90(3) 13_666 16_546 ? AL2 AL1 Ca1 65.278(16) 4_664 16_546 ? AL1 AL1 Ca1 114.77(3) 3_665 16_546 ? AL1 AL1 Ca1 64.05(3) 2_655 16_546 ? Ca2 AL1 Ca1 63.574(17) 16_556 16_546 ? Ca2 AL1 Ca1 117.10(3) . 16_546 ? AL1 AL1 Ca1 65.23(3) 3 1_545 ? AL1 AL1 Ca1 115.95(3) 2 1_545 ? AL2 AL1 Ca1 65.278(16) 13_666 1_545 ? AL2 AL1 Ca1 113.90(3) 4_664 1_545 ? AL1 AL1 Ca1 114.77(3) 3_665 1_545 ? AL1 AL1 Ca1 64.05(3) 2_655 1_545 ? Ca2 AL1 Ca1 117.10(3) 16_556 1_545 ? Ca2 AL1 Ca1 63.574(17) . 1_545 ? Ca1 AL1 Ca1 62.12(3) 16_546 1_545 ? AL1 AL1 Ca1 115.95(3) 3 . ? AL1 AL1 Ca1 65.23(3) 2 . ? AL2 AL1 Ca1 65.278(16) 13_666 . ? AL2 AL1 Ca1 113.90(3) 4_664 . ? AL1 AL1 Ca1 64.05(3) 3_665 . ? AL1 AL1 Ca1 114.77(3) 2_655 . ? Ca2 AL1 Ca1 117.10(3) 16_556 . ? Ca2 AL1 Ca1 63.574(17) . . ? Ca1 AL1 Ca1 178.76(6) 16_546 . ? Ca1 AL1 Ca1 117.87(3) 1_545 . ? AL1 AL1 Ca1 115.95(3) 3 16_556 ? AL1 AL1 Ca1 65.23(3) 2 16_556 ? AL2 AL1 Ca1 113.90(3) 13_666 16_556 ? AL2 AL1 Ca1 65.278(16) 4_664 16_556 ? AL1 AL1 Ca1 64.05(3) 3_665 16_556 ? AL1 AL1 Ca1 114.77(3) 2_655 16_556 ? Ca2 AL1 Ca1 63.574(17) 16_556 16_556 ? Ca2 AL1 Ca1 117.10(3) . 16_556 ? Ca1 AL1 Ca1 117.87(3) 16_546 16_556 ? Ca1 AL1 Ca1 178.76(6) 1_545 16_556 ? Ca1 AL1 Ca1 62.12(3) . 16_556 ? AL1 AL2 AL1 62.92(5) 14_566 13_666 ? AL1 AL2 AL1 62.92(5) 14_566 15_556 ? AL1 AL2 AL1 62.92(6) 13_666 15_556 ? AL1 AL2 Mg1 119.09(2) 14_566 . ? AL1 AL2 Mg1 177.50(5) 13_666 . ? AL1 AL2 Mg1 119.09(2) 15_556 . ? AL1 AL2 Mg1 119.09(2) 14_566 3_565 ? AL1 AL2 Mg1 119.09(2) 13_666 3_565 ? AL1 AL2 Mg1 177.50(5) 15_556 3_565 ? Mg1 AL2 Mg1 58.86(3) . 3_565 ? AL1 AL2 Mg1 177.50(5) 14_566 2_665 ? AL1 AL2 Mg1 119.09(2) 13_666 2_665 ? AL1 AL2 Mg1 119.09(2) 15_556 2_665 ? Mg1 AL2 Mg1 58.86(3) . 2_665 ? Mg1 AL2 Mg1 58.86(3) 3_565 2_665 ? AL1 AL2 Ca1 65.17(3) 14_566 13_676 ? AL1 AL2 Ca1 65.17(3) 13_666 13_676 ? AL1 AL2 Ca1 118.26(6) 15_556 13_676 ? Mg1 AL2 Ca1 113.98(4) . 13_676 ? Mg1 AL2 Ca1 64.24(2) 3_565 13_676 ? Mg1 AL2 Ca1 113.98(4) 2_665 13_676 ? AL1 AL2 Ca1 65.17(3) 14_566 13_566 ? AL1 AL2 Ca1 118.26(6) 13_666 13_566 ? AL1 AL2 Ca1 65.17(3) 15_556 13_566 ? Mg1 AL2 Ca1 64.24(2) . 13_566 ? Mg1 AL2 Ca1 113.98(4) 3_565 13_566 ? Mg1 AL2 Ca1 113.98(4) 2_665 13_566 ? Ca1 AL2 Ca1 117.701(19) 13_676 13_566 ? AL1 AL2 Ca1 118.26(6) 14_566 13_666 ? AL1 AL2 Ca1 65.17(3) 13_666 13_666 ? AL1 AL2 Ca1 65.17(3) 15_556 13_666 ? Mg1 AL2 Ca1 113.98(4) . 13_666 ? Mg1 AL2 Ca1 113.98(4) 3_565 13_666 ? Mg1 AL2 Ca1 64.24(2) 2_665 13_666 ? Ca1 AL2 Ca1 117.701(19) 13_676 13_666 ? Ca1 AL2 Ca1 117.701(19) 13_566 13_666 ? AL1 AL2 Ca2 64.15(3) 14_566 13_566 ? AL1 AL2 Ca2 116.79(4) 13_666 13_566 ? AL1 AL2 Ca2 116.79(4) 15_556 13_566 ? Mg1 AL2 Ca2 64.00(3) . 13_566 ? Mg1 AL2 Ca2 64.00(3) 3_565 13_566 ? Mg1 AL2 Ca2 113.36(6) 2_665 13_566 ? Ca1 AL2 Ca2 62.940(6) 13_676 13_566 ? Ca1 AL2 Ca2 62.940(6) 13_566 13_566 ? Ca1 AL2 Ca2 177.60(7) 13_666 13_566 ? AL1 AL2 Ca2 116.79(4) 14_566 13_556 ? AL1 AL2 Ca2 116.79(4) 13_666 13_556 ? AL1 AL2 Ca2 64.15(4) 15_556 13_556 ? Mg1 AL2 Ca2 64.00(3) . 13_556 ? Mg1 AL2 Ca2 113.36(6) 3_565 13_556 ? Mg1 AL2 Ca2 64.00(3) 2_665 13_556 ? Ca1 AL2 Ca2 177.60(7) 13_676 13_556 ? Ca1 AL2 Ca2 62.940(6) 13_566 13_556 ? Ca1 AL2 Ca2 62.940(6) 13_666 13_556 ? Ca2 AL2 Ca2 116.32(2) 13_566 13_556 ? AL1 AL2 Ca2 116.79(4) 14_566 13_666 ? AL1 AL2 Ca2 64.15(4) 13_666 13_666 ? AL1 AL2 Ca2 116.79(4) 15_556 13_666 ? Mg1 AL2 Ca2 113.36(6) . 13_666 ? Mg1 AL2 Ca2 64.00(3) 3_565 13_666 ? Mg1 AL2 Ca2 64.00(3) 2_665 13_666 ? Ca1 AL2 Ca2 62.940(6) 13_676 13_666 ? Ca1 AL2 Ca2 177.60(7) 13_566 13_666 ? Ca1 AL2 Ca2 62.940(6) 13_666 13_666 ? Ca2 AL2 Ca2 116.32(2) 13_566 13_666 ? Ca2 AL2 Ca2 116.32(2) 13_556 13_666 ? Mg1 Mg1 Mg1 180.0 3_565 3_455 ? Mg1 Mg1 Mg1 60.0 3_565 2_665 ? Mg1 Mg1 Mg1 120.0 3_455 2_665 ? Mg1 Mg1 Mg1 120.0 3_565 2_565 ? Mg1 Mg1 Mg1 60.0 3_455 2_565 ? Mg1 Mg1 Mg1 180.0 2_665 2_565 ? Mg1 Mg1 AL2 119.428(15) 3_565 13_566 ? Mg1 Mg1 AL2 60.572(15) 3_455 13_566 ? Mg1 Mg1 AL2 119.428(15) 2_665 13_566 ? Mg1 Mg1 AL2 60.572(15) 2_565 13_566 ? Mg1 Mg1 AL2 60.572(15) 3_565 . ? Mg1 Mg1 AL2 119.428(15) 3_455 . ? Mg1 Mg1 AL2 60.572(15) 2_665 . ? Mg1 Mg1 AL2 119.428(15) 2_565 . ? AL2 Mg1 AL2 180.0 13_566 . ? Mg1 Mg1 Ca1 115.315(8) 3_565 13_566 ? Mg1 Mg1 Ca1 64.685(8) 3_455 13_566 ? Mg1 Mg1 Ca1 115.315(8) 2_665 13_566 ? Mg1 Mg1 Ca1 64.685(8) 2_565 13_566 ? AL2 Mg1 Ca1 115.85(2) 13_566 13_566 ? AL2 Mg1 Ca1 64.15(2) . 13_566 ? Mg1 Mg1 Ca1 64.685(8) 3_565 . ? Mg1 Mg1 Ca1 115.315(8) 3_455 . ? Mg1 Mg1 Ca1 64.685(8) 2_665 . ? Mg1 Mg1 Ca1 115.315(8) 2_565 . ? AL2 Mg1 Ca1 64.15(2) 13_566 . ? AL2 Mg1 Ca1 115.85(2) . . ? Ca1 Mg1 Ca1 180.0 13_566 . ? Mg1 Mg1 Ca2 115.278(5) 3_565 . ? Mg1 Mg1 Ca2 64.722(5) 3_455 . ? Mg1 Mg1 Ca2 64.722(5) 2_665 . ? Mg1 Mg1 Ca2 115.278(5) 2_565 . ? AL2 Mg1 Ca2 64.633(12) 13_566 . ? AL2 Mg1 Ca2 115.367(12) . . ? Ca1 Mg1 Ca2 116.899(15) 13_566 . ? Ca1 Mg1 Ca2 63.101(15) . . ? Mg1 Mg1 Ca2 64.722(5) 3_565 13_566 ? Mg1 Mg1 Ca2 115.278(5) 3_455 13_566 ? Mg1 Mg1 Ca2 115.278(5) 2_665 13_566 ? Mg1 Mg1 Ca2 64.722(5) 2_565 13_566 ? AL2 Mg1 Ca2 115.367(12) 13_566 13_566 ? AL2 Mg1 Ca2 64.633(12) . 13_566 ? Ca1 Mg1 Ca2 63.101(15) 13_566 13_566 ? Ca1 Mg1 Ca2 116.899(15) . 13_566 ? Ca2 Mg1 Ca2 180.0 . 13_566 ? Mg1 Mg1 Ca2 64.722(5) 3_565 1_565 ? Mg1 Mg1 Ca2 115.278(5) 3_455 1_565 ? Mg1 Mg1 Ca2 115.278(5) 2_665 1_565 ? Mg1 Mg1 Ca2 64.722(5) 2_565 1_565 ? AL2 Mg1 Ca2 64.633(12) 13_566 1_565 ? AL2 Mg1 Ca2 115.367(12) . 1_565 ? Ca1 Mg1 Ca2 116.899(15) 13_566 1_565 ? Ca1 Mg1 Ca2 63.101(15) . 1_565 ? Ca2 Mg1 Ca2 117.30(3) . 1_565 ? Ca2 Mg1 Ca2 62.70(3) 13_566 1_565 ? Mg1 Mg1 Ca2 115.278(5) 3_565 13_556 ? Mg1 Mg1 Ca2 64.722(5) 3_455 13_556 ? Mg1 Mg1 Ca2 64.722(5) 2_665 13_556 ? Mg1 Mg1 Ca2 115.278(5) 2_565 13_556 ? AL2 Mg1 Ca2 115.367(12) 13_566 13_556 ? AL2 Mg1 Ca2 64.633(12) . 13_556 ? Ca1 Mg1 Ca2 63.101(15) 13_566 13_556 ? Ca1 Mg1 Ca2 116.899(15) . 13_556 ? Ca2 Mg1 Ca2 62.70(3) . 13_556 ? Ca2 Mg1 Ca2 117.30(3) 13_566 13_556 ? Ca2 Mg1 Ca2 180.0 1_565 13_556 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.09 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.500 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.108 #===END