data_shelx _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common claringbullite _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'CU4 O6 CL1 F1' _chemical_formula_weight 404.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.3201 1.2651 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 11.5364(2) _cell_length_b 9.16830(10) _cell_length_c 6.67250(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 705.745(18) _cell_formula_units_Z 4 _cell_measurement_temperature 249.9(7) _cell_measurement_reflns_used 6481 _cell_measurement_theta_min 4.6500 _cell_measurement_theta_max 31.2520 _exptl_crystal_description 'subhedral tabular crystal' _exptl_crystal_colour 'dark blue _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.175 _exptl_crystal_size_min 0.065 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 12.268 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.23a (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Xcalibur EOS detector Agilent Technologies' _diffrn_measurement_method '1K CCD-based area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 120 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2308 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 31.72 _reflns_number_total 2308 _reflns_number_gt 1914 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)' _computing_data_reduction 'CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Crystalmaker' _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. ; _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^)+(0.0767P)^2^+0.7238P] 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 0.0293(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2308 _refine_ls_number_parameters 67 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.1235 _refine_ls_wR_factor_gt 0.1220 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 Cu1 Cu 0.18550(6) 0.2500 0.05967(10) 0.0078(2) Uiso 0.754(4) 2 d SP . . Cu4 Cu 0.1313(3) 0.2500 0.0037(4) 0.0078(2) Uiso 0.172(2) 2 d SP . . Cu5 Cu 0.1824(10) 0.2500 -0.0422(16) 0.0078(2) Uiso 0.0513(17) 2 d SP . . Cu2 Cu 0.0000 0.0000 0.0000 0.0116(2) Uani 1 2 d S . . Cu3 Cu 0.25095(2) 0.50975(4) 0.24676(4) 0.01134(17) Uani 1 1 d . . . F F 0.4986(2) 0.2500 0.0061(3) 0.0178(6) Uani 1 2 d S . . O1 O 0.29786(18) 0.0929(2) 0.0015(2) 0.0097(4) Uani 1 1 d . . . O2 O 0.40111(17) 0.5892(2) 0.3028(3) 0.0116(4) Uani 1 1 d . . . O3 O 0.10316(16) 0.0916(2) 0.1980(3) 0.0093(4) Uani 1 1 d . . . Cl Cl 0.33019(14) 0.2500 0.50627(15) 0.0199(2) Uani 1 2 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 Cu2 0.0083(3) 0.0187(4) 0.0077(3) -0.00072(14) 0.00032(13) -0.00440(18) Cu3 0.0083(3) 0.0174(3) 0.0083(3) -0.00382(11) 0.00015(12) -0.00205(14) F 0.0152(17) 0.0232(15) 0.0149(16) 0.000 -0.0017(8) 0.000 O1 0.0106(11) 0.0130(11) 0.0055(9) -0.0005(6) 0.0004(5) 0.0000(9) O2 0.0083(9) 0.0169(10) 0.0096(9) 0.0021(7) -0.0035(6) -0.0027(8) O3 0.0078(9) 0.0127(9) 0.0076(9) 0.0009(6) -0.0018(6) 0.0008(8) Cl 0.0228(7) 0.0164(5) 0.0204(6) 0.000 -0.0001(3) 0.000 _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 Cu1 Cu5 0.681(11) . ? Cu1 Cu4 0.728(3) . ? Cu1 O3 1.9657(19) . ? Cu1 O3 1.9657(19) 8_565 ? Cu1 O1 1.976(2) 8_565 ? Cu1 O1 1.976(2) . ? Cu1 Cu3 2.7928(5) . ? Cu1 Cu3 2.7928(5) 8_565 ? Cu4 Cu5 0.664(10) . ? Cu4 O3 1.974(3) 8_565 ? Cu4 O3 1.974(3) . ? Cu4 O2 2.028(3) 7_655 ? Cu4 O2 2.028(3) 2_564 ? Cu4 O1 2.401(4) 8_565 ? Cu4 O1 2.401(4) . ? Cu4 Cu2 2.748(2) . ? Cu4 Cu2 2.748(2) 4 ? Cu5 O1 1.983(8) 8_565 ? Cu5 O1 1.983(8) . ? Cu5 O2 2.042(8) 7_655 ? Cu5 O2 2.042(8) 2_564 ? Cu5 O3 2.348(9) 8_565 ? Cu5 O3 2.348(9) . ? Cu5 Cu3 2.725(6) 7_655 ? Cu5 Cu3 2.725(6) 2_564 ? Cu2 O2 1.9242(19) 3_455 ? Cu2 O2 1.9242(19) 7_655 ? Cu2 O3 1.9663(18) . ? Cu2 O3 1.9663(18) 5 ? Cu2 Cu4 2.748(2) 5 ? Cu3 O2 1.916(2) . ? Cu3 O1 1.9461(17) 7_666 ? Cu3 O1 1.9638(18) 8_565 ? Cu3 O3 1.9686(19) 8_565 ? Cu3 Cu5 2.725(6) 2_565 ? O1 Cu3 1.9461(17) 7_655 ? O1 Cu3 1.9638(18) 8_565 ? O2 Cu2 1.9242(19) 3 ? O2 Cu4 2.028(3) 2_565 ? O2 Cu5 2.042(8) 2_565 ? O3 Cu3 1.9686(19) 8_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 Cu5 Cu1 Cu4 56.1(9) . . ? Cu5 Cu1 O3 116.3(5) . . ? Cu4 Cu1 O3 79.98(16) . . ? Cu5 Cu1 O3 116.3(5) . 8_565 ? Cu4 Cu1 O3 79.98(16) . 8_565 ? O3 Cu1 O3 95.28(11) . 8_565 ? Cu5 Cu1 O1 80.7(6) . 8_565 ? Cu4 Cu1 O1 117.54(15) . 8_565 ? O3 Cu1 O1 161.39(8) . 8_565 ? O3 Cu1 O1 82.56(8) 8_565 8_565 ? Cu5 Cu1 O1 80.7(6) . . ? Cu4 Cu1 O1 117.54(15) . . ? O3 Cu1 O1 82.56(8) . . ? O3 Cu1 O1 161.39(8) 8_565 . ? O1 Cu1 O1 93.58(13) 8_565 . ? Cu5 Cu1 Cu3 117.4(3) . . ? Cu4 Cu1 Cu3 117.47(6) . . ? O3 Cu1 Cu3 123.43(6) . . ? O3 Cu1 Cu3 44.82(6) 8_565 . ? O1 Cu1 Cu3 44.68(5) 8_565 . ? O1 Cu1 Cu3 122.14(7) . . ? Cu5 Cu1 Cu3 117.4(3) . 8_565 ? Cu4 Cu1 Cu3 117.47(6) . 8_565 ? O3 Cu1 Cu3 44.82(6) . 8_565 ? O3 Cu1 Cu3 123.43(6) 8_565 8_565 ? O1 Cu1 Cu3 122.14(7) 8_565 8_565 ? O1 Cu1 Cu3 44.68(5) . 8_565 ? Cu3 Cu1 Cu3 117.01(3) . 8_565 ? Cu5 Cu4 Cu1 58.3(10) . . ? Cu5 Cu4 O3 116.7(6) . 8_565 ? Cu1 Cu4 O3 78.71(15) . 8_565 ? Cu5 Cu4 O3 116.7(6) . . ? Cu1 Cu4 O3 78.71(15) . . ? O3 Cu4 O3 94.76(15) 8_565 . ? Cu5 Cu4 O2 81.9(6) . 7_655 ? Cu1 Cu4 O2 119.8(2) . 7_655 ? O3 Cu4 O2 159.9(2) 8_565 7_655 ? O3 Cu4 O2 82.47(9) . 7_655 ? Cu5 Cu4 O2 81.9(6) . 2_564 ? Cu1 Cu4 O2 119.8(2) . 2_564 ? O3 Cu4 O2 82.47(9) 8_565 2_564 ? O3 Cu4 O2 159.9(2) . 2_564 ? O2 Cu4 O2 93.30(15) 7_655 2_564 ? Cu5 Cu4 O1 44.5(5) . 8_565 ? Cu1 Cu4 O1 46.86(15) . 8_565 ? O3 Cu4 O1 72.19(10) 8_565 8_565 ? O3 Cu4 O1 125.24(16) . 8_565 ? O2 Cu4 O1 125.43(17) 7_655 8_565 ? O2 Cu4 O1 72.99(10) 2_564 8_565 ? Cu5 Cu4 O1 44.5(5) . . ? Cu1 Cu4 O1 46.86(15) . . ? O3 Cu4 O1 125.24(16) 8_565 . ? O3 Cu4 O1 72.19(10) . . ? O2 Cu4 O1 72.99(10) 7_655 . ? O2 Cu4 O1 125.43(17) 2_564 . ? O1 Cu4 O1 73.71(15) 8_565 . ? Cu5 Cu4 Cu2 119.0(3) . . ? Cu1 Cu4 Cu2 118.55(8) . . ? O3 Cu4 Cu2 121.94(16) 8_565 . ? O3 Cu4 Cu2 45.68(7) . . ? O2 Cu4 Cu2 44.42(7) 7_655 . ? O2 Cu4 Cu2 119.94(15) 2_564 . ? O1 Cu4 Cu2 160.30(13) 8_565 . ? O1 Cu4 Cu2 86.60(5) . . ? Cu5 Cu4 Cu2 119.0(3) . 4 ? Cu1 Cu4 Cu2 118.55(8) . 4 ? O3 Cu4 Cu2 45.68(7) 8_565 4 ? O3 Cu4 Cu2 121.94(16) . 4 ? O2 Cu4 Cu2 119.94(15) 7_655 4 ? O2 Cu4 Cu2 44.42(7) 2_564 4 ? O1 Cu4 Cu2 86.60(5) 8_565 4 ? O1 Cu4 Cu2 160.30(13) . 4 ? Cu2 Cu4 Cu2 113.07(13) . 4 ? Cu4 Cu5 Cu1 65.5(10) . . ? Cu4 Cu5 O1 121.9(6) . 8_565 ? Cu1 Cu5 O1 79.5(6) . 8_565 ? Cu4 Cu5 O1 121.9(6) . . ? Cu1 Cu5 O1 79.5(6) . . ? O1 Cu5 O1 93.1(5) 8_565 . ? Cu4 Cu5 O2 79.3(7) . 7_655 ? Cu1 Cu5 O2 122.0(6) . 7_655 ? O1 Cu5 O2 156.3(6) 8_565 7_655 ? O1 Cu5 O2 82.36(14) . 7_655 ? Cu4 Cu5 O2 79.3(7) . 2_564 ? Cu1 Cu5 O2 122.0(6) . 2_564 ? O1 Cu5 O2 82.36(14) 8_565 2_564 ? O1 Cu5 O2 156.3(6) . 2_564 ? O2 Cu5 O2 92.4(5) 7_655 2_564 ? Cu4 Cu5 O3 48.7(5) . 8_565 ? Cu1 Cu5 O3 48.6(5) . 8_565 ? O1 Cu5 O3 73.2(2) 8_565 8_565 ? O1 Cu5 O3 127.6(5) . 8_565 ? O2 Cu5 O3 127.5(5) 7_655 8_565 ? O2 Cu5 O3 73.5(2) 2_564 8_565 ? Cu4 Cu5 O3 48.7(5) . . ? Cu1 Cu5 O3 48.6(5) . . ? O1 Cu5 O3 127.6(5) 8_565 . ? O1 Cu5 O3 73.2(2) . . ? O2 Cu5 O3 73.5(2) 7_655 . ? O2 Cu5 O3 127.5(5) 2_564 . ? O3 Cu5 O3 76.4(3) 8_565 . ? Cu4 Cu5 Cu3 119.2(5) . 7_655 ? Cu1 Cu5 Cu3 120.1(4) . 7_655 ? O1 Cu5 Cu3 118.3(5) 8_565 7_655 ? O1 Cu5 Cu3 45.54(14) . 7_655 ? O2 Cu5 Cu3 44.60(14) 7_655 7_655 ? O2 Cu5 Cu3 117.1(4) 2_564 7_655 ? O3 Cu5 Cu3 164.3(4) 8_565 7_655 ? O3 Cu5 Cu3 87.85(5) . 7_655 ? Cu4 Cu5 Cu3 119.2(5) . 2_564 ? Cu1 Cu5 Cu3 120.1(4) . 2_564 ? O1 Cu5 Cu3 45.54(14) 8_565 2_564 ? O1 Cu5 Cu3 118.3(5) . 2_564 ? O2 Cu5 Cu3 117.1(4) 7_655 2_564 ? O2 Cu5 Cu3 44.60(14) 2_564 2_564 ? O3 Cu5 Cu3 87.85(5) 8_565 2_564 ? O3 Cu5 Cu3 164.3(4) . 2_564 ? Cu3 Cu5 Cu3 107.9(4) 7_655 2_564 ? O2 Cu2 O2 180.00(16) 3_455 7_655 ? O2 Cu2 O3 94.63(9) 3_455 . ? O2 Cu2 O3 85.37(9) 7_655 . ? O2 Cu2 O3 85.37(9) 3_455 5 ? O2 Cu2 O3 94.63(9) 7_655 5 ? O3 Cu2 O3 180.00(12) . 5 ? O2 Cu2 Cu4 132.48(8) 3_455 . ? O2 Cu2 Cu4 47.52(8) 7_655 . ? O3 Cu2 Cu4 45.90(7) . . ? O3 Cu2 Cu4 134.10(7) 5 . ? O2 Cu2 Cu4 47.52(8) 3_455 5 ? O2 Cu2 Cu4 132.48(8) 7_655 5 ? O3 Cu2 Cu4 134.10(7) . 5 ? O3 Cu2 Cu4 45.90(7) 5 5 ? Cu4 Cu2 Cu4 180.0 . 5 ? O2 Cu3 O1 86.70(8) . 7_666 ? O2 Cu3 O1 95.48(8) . 8_565 ? O1 Cu3 O1 174.43(4) 7_666 8_565 ? O2 Cu3 O3 174.06(7) . 8_565 ? O1 Cu3 O3 94.51(8) 7_666 8_565 ? O1 Cu3 O3 82.81(8) 8_565 8_565 ? O2 Cu3 Cu5 48.5(2) . 2_565 ? O1 Cu3 Cu5 46.7(2) 7_666 2_565 ? O1 Cu3 Cu5 137.7(2) 8_565 2_565 ? O3 Cu3 Cu5 135.3(2) 8_565 2_565 ? O2 Cu3 Cu1 130.98(6) . . ? O1 Cu3 Cu1 130.26(7) 7_666 . ? O1 Cu3 Cu1 45.04(7) 8_565 . ? O3 Cu3 Cu1 44.73(6) 8_565 . ? Cu5 Cu3 Cu1 175.22(19) 2_565 . ? Cu3 O1 Cu3 117.41(11) 7_655 8_565 ? Cu3 O1 Cu1 105.50(9) 7_655 . ? Cu3 O1 Cu1 90.28(8) 8_565 . ? Cu3 O1 Cu5 87.8(3) 7_655 . ? Cu3 O1 Cu5 106.6(3) 8_565 . ? Cu1 O1 Cu5 19.8(3) . . ? Cu3 O1 Cu4 90.50(9) 7_655 . ? Cu3 O1 Cu4 93.55(10) 8_565 . ? Cu1 O1 Cu4 15.60(5) . . ? Cu5 O1 Cu4 13.6(3) . . ? Cu3 O2 Cu2 120.52(10) . 3 ? Cu3 O2 Cu4 103.80(14) . 2_565 ? Cu2 O2 Cu4 88.06(11) 3 2_565 ? Cu3 O2 Cu5 86.9(3) . 2_565 ? Cu2 O2 Cu5 103.9(3) 3 2_565 ? Cu4 O2 Cu5 18.8(3) 2_565 2_565 ? Cu1 O3 Cu2 107.01(8) . . ? Cu1 O3 Cu3 90.45(8) . 8_565 ? Cu2 O3 Cu3 115.71(9) . 8_565 ? Cu1 O3 Cu4 21.31(10) . . ? Cu2 O3 Cu4 88.42(11) . . ? Cu3 O3 Cu4 108.26(14) 8_565 . ? Cu1 O3 Cu5 15.1(2) . . ? Cu2 O3 Cu5 92.4(3) . . ? Cu3 O3 Cu5 93.9(3) 8_565 . ? Cu4 O3 Cu5 14.6(2) . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 2.197 _refine_diff_density_min -1.297 _refine_diff_density_rms 0.284