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 11.5276(2) _cell_length_b 9.16410(10) _cell_length_c 6.67360(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 705.000(18) _cell_formula_units_Z 4 _cell_measurement_temperature 200.00(14) _cell_measurement_reflns_used 7023 _cell_measurement_theta_min 3.7790 _cell_measurement_theta_max 31.6110 _exptl_crystal_description 'subhedral tabular crystal' _exptl_crystal_colour 'dark green' _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 3.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 12.281 _exptl_absorpt_correction_T_min 0.84802 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 120 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2301 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0137 _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 2301 _reflns_number_gt 1991 _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^)+(0.0655P)^2^+2.4904P] 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 0.0224(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2301 _refine_ls_number_parameters 64 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _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 Cu1 Cu 0.18540(6) 0.2500 0.06025(9) 0.0067(2) Uiso 0.872(4) 2 d SP . . Cu4 Cu 0.1347(6) 0.2500 0.0042(8) 0.0067(2) Uiso 0.096(2) 2 d SP . . Cu2 Cu 0.0000 0.0000 0.0000 0.00842(18) Uani 1 2 d S . . Cu3 Cu 0.25102(3) 0.51190(5) 0.24585(5) 0.00856(16) Uani 1 1 d . . . F F 0.4977(3) 0.2500 0.0072(4) 0.0137(6) Uani 1 2 d S . . O1 O 0.2977(2) 0.0931(3) 0.0018(3) 0.0074(5) Uani 1 1 d . . . O2 O 0.4014(2) 0.5881(3) 0.3025(3) 0.0093(4) Uani 1 1 d . . . O3 O 0.10354(19) 0.0910(2) 0.1986(3) 0.0073(4) Uani 1 1 d . . . Cl Cl 0.32892(13) 0.2500 0.50791(16) 0.0157(3) 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 0.0067(3) 0.0131(3) 0.0055(3) -0.00034(16) 0.00021(15) -0.0036(2) Cu3 0.0064(3) 0.0131(3) 0.0062(3) -0.00310(12) 0.00013(12) -0.00147(14) F 0.0119(17) 0.0188(15) 0.0105(15) 0.000 -0.0014(9) 0.000 O1 0.0084(11) 0.0095(11) 0.0042(9) -0.0006(6) 0.0003(6) -0.0005(10) O2 0.0067(9) 0.0135(10) 0.0078(10) 0.0023(8) -0.0030(7) -0.0018(9) O3 0.0060(9) 0.0104(10) 0.0055(9) 0.0004(7) -0.0011(7) 0.0002(8) Cl 0.0190(7) 0.0128(5) 0.0153(5) 0.000 0.0001(4) 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 Cu4 0.694(6) . ? Cu1 O3 1.966(2) . ? Cu1 O3 1.966(2) 8_565 ? Cu1 O1 1.974(2) 8_565 ? Cu1 O1 1.974(2) . ? Cu1 Cu3 2.8048(5) . ? Cu1 Cu3 2.8048(5) 8_565 ? Cu4 O3 1.984(4) 8_565 ? Cu4 O3 1.984(4) . ? Cu4 O2 2.046(4) 7_655 ? Cu4 O2 2.046(4) 2_564 ? Cu4 O1 2.366(6) 8_565 ? Cu4 O1 2.366(6) . ? Cu4 Cu2 2.768(4) . ? Cu4 Cu2 2.768(4) 4 ? Cu2 O2 1.919(2) 7_655 ? Cu2 O2 1.919(2) 3_455 ? Cu2 O3 1.969(2) 5 ? Cu2 O3 1.969(2) . ? Cu2 Cu4 2.768(4) 5 ? Cu3 O2 1.907(2) . ? Cu3 O1 1.946(2) 7_666 ? Cu3 O1 1.967(2) 8_565 ? Cu3 O3 1.970(2) 8_565 ? O1 Cu3 1.946(2) 7_655 ? O1 Cu3 1.967(2) 8_565 ? O2 Cu2 1.919(2) 3 ? O2 Cu4 2.046(4) 2_565 ? O3 Cu3 1.970(2) 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 Cu4 Cu1 O3 81.3(3) . . ? Cu4 Cu1 O3 81.3(3) . 8_565 ? O3 Cu1 O3 95.63(13) . 8_565 ? Cu4 Cu1 O1 116.5(3) . 8_565 ? O3 Cu1 O1 161.34(9) . 8_565 ? O3 Cu1 O1 82.42(9) 8_565 8_565 ? Cu4 Cu1 O1 116.5(3) . . ? O3 Cu1 O1 82.42(9) . . ? O3 Cu1 O1 161.34(9) 8_565 . ? O1 Cu1 O1 93.50(14) 8_565 . ? Cu4 Cu1 Cu3 117.72(11) . . ? O3 Cu1 Cu3 123.78(7) . . ? O3 Cu1 Cu3 44.60(6) 8_565 . ? O1 Cu1 Cu3 44.53(6) 8_565 . ? O1 Cu1 Cu3 122.25(7) . . ? Cu4 Cu1 Cu3 117.72(11) . 8_565 ? O3 Cu1 Cu3 44.60(6) . 8_565 ? O3 Cu1 Cu3 123.78(7) 8_565 8_565 ? O1 Cu1 Cu3 122.25(7) 8_565 8_565 ? O1 Cu1 Cu3 44.53(6) . 8_565 ? Cu3 Cu1 Cu3 117.68(3) . 8_565 ? Cu1 Cu4 O3 78.5(3) . 8_565 ? Cu1 Cu4 O3 78.5(3) . . ? O3 Cu4 O3 94.5(2) 8_565 . ? Cu1 Cu4 O2 121.7(3) . 7_655 ? O3 Cu4 O2 157.8(4) 8_565 7_655 ? O3 Cu4 O2 82.01(11) . 7_655 ? Cu1 Cu4 O2 121.7(3) . 2_564 ? O3 Cu4 O2 82.01(11) 8_565 2_564 ? O3 Cu4 O2 157.8(4) . 2_564 ? O2 Cu4 O2 93.0(3) 7_655 2_564 ? Cu1 Cu4 O1 48.3(3) . 8_565 ? O3 Cu4 O1 72.66(15) 8_565 8_565 ? O3 Cu4 O1 126.5(3) . 8_565 ? O2 Cu4 O1 126.7(3) 7_655 8_565 ? O2 Cu4 O1 73.52(13) 2_564 8_565 ? Cu1 Cu4 O1 48.3(3) . . ? O3 Cu4 O1 126.5(3) 8_565 . ? O3 Cu4 O1 72.66(15) . . ? O2 Cu4 O1 73.52(13) 7_655 . ? O2 Cu4 O1 126.7(3) 2_564 . ? O1 Cu4 O1 74.8(2) 8_565 . ? Cu1 Cu4 Cu2 118.55(18) . . ? O3 Cu4 Cu2 120.9(3) 8_565 . ? O3 Cu4 Cu2 45.35(10) . . ? O2 Cu4 Cu2 43.87(10) 7_655 . ? O2 Cu4 Cu2 118.7(3) 2_564 . ? O1 Cu4 Cu2 161.5(2) 8_565 . ? O1 Cu4 Cu2 86.71(6) . . ? Cu1 Cu4 Cu2 118.55(18) . 4 ? O3 Cu4 Cu2 45.35(10) 8_565 4 ? O3 Cu4 Cu2 120.9(3) . 4 ? O2 Cu4 Cu2 118.7(3) 7_655 4 ? O2 Cu4 Cu2 43.87(10) 2_564 4 ? O1 Cu4 Cu2 86.71(6) 8_565 4 ? O1 Cu4 Cu2 161.5(2) . 4 ? Cu2 Cu4 Cu2 111.7(2) . 4 ? O2 Cu2 O2 180.00(19) 7_655 3_455 ? O2 Cu2 O3 94.31(9) 7_655 5 ? O2 Cu2 O3 85.69(9) 3_455 5 ? O2 Cu2 O3 85.69(9) 7_655 . ? O2 Cu2 O3 94.31(9) 3_455 . ? O3 Cu2 O3 180.00(18) 5 . ? O2 Cu2 Cu4 47.64(12) 7_655 . ? O2 Cu2 Cu4 132.36(12) 3_455 . ? O3 Cu2 Cu4 134.23(12) 5 . ? O3 Cu2 Cu4 45.77(12) . . ? O2 Cu2 Cu4 132.36(12) 7_655 5 ? O2 Cu2 Cu4 47.64(12) 3_455 5 ? O3 Cu2 Cu4 45.77(12) 5 5 ? O3 Cu2 Cu4 134.23(12) . 5 ? Cu4 Cu2 Cu4 180.0(2) . 5 ? O2 Cu3 O1 87.03(10) . 7_666 ? O2 Cu3 O1 95.44(10) . 8_565 ? O1 Cu3 O1 173.20(5) 7_666 8_565 ? O2 Cu3 O3 172.69(9) . 8_565 ? O1 Cu3 O3 94.28(9) 7_666 8_565 ? O1 Cu3 O3 82.49(9) 8_565 8_565 ? O2 Cu3 Cu1 130.26(7) . . ? O1 Cu3 Cu1 129.58(8) 7_666 . ? O1 Cu3 Cu1 44.71(7) 8_565 . ? O3 Cu3 Cu1 44.49(6) 8_565 . ? Cu3 O1 Cu3 117.42(12) 7_655 8_565 ? Cu3 O1 Cu1 105.24(11) 7_655 . ? Cu3 O1 Cu1 90.75(9) 8_565 . ? Cu3 O1 Cu4 90.53(15) 7_655 . ? Cu3 O1 Cu4 94.26(14) 8_565 . ? Cu1 O1 Cu4 15.22(11) . . ? Cu3 O2 Cu2 121.38(11) . 3 ? Cu3 O2 Cu4 102.2(2) . 2_565 ? Cu2 O2 Cu4 88.49(16) 3 2_565 ? Cu1 O3 Cu2 106.78(9) . . ? Cu1 O3 Cu3 90.91(9) . 8_565 ? Cu2 O3 Cu3 115.34(11) . 8_565 ? Cu1 O3 Cu4 20.24(19) . . ? Cu2 O3 Cu4 88.88(18) . . ? Cu3 O3 Cu4 107.5(2) 8_565 . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 2.091 _refine_diff_density_min -1.340 _refine_diff_density_rms 0.302