Demartin_AM-12-062
 
data_argesite
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'H23.16 Bi3 Br1.42 Cl14.58 K1.21 N5.79'
_chemical_formula_weight          1409.05
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 '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'
 'Bi'  'Bi'  -4.1077  10.2566
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'K'  'K'   0.2009   0.2494
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Br'  'Br'  -0.2901   2.4595
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            trigonal
_symmetry_space_group_name_H-M    R-3c
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-y, x-y, z'
 'y, x, -z+1/2'
 '-x+y, -x, z'
 '-x, -x+y, -z+1/2'
 'x-y, -y, -z+1/2'
 'x+2/3, y+1/3, z+1/3'
 '-y+2/3, x-y+1/3, z+1/3'
 'y+2/3, x+1/3, -z+5/6'
 '-x+y+2/3, -x+1/3, z+1/3'
 '-x+2/3, -x+y+1/3, -z+5/6'
 'x-y+2/3, -y+1/3, -z+5/6'
 'x+1/3, y+2/3, z+2/3'
 '-y+1/3, x-y+2/3, z+2/3'
 'y+1/3, x+2/3, -z+7/6'
 '-x+y+1/3, -x+2/3, z+2/3'
 '-x+1/3, -x+y+2/3, -z+7/6'
 'x-y+1/3, -y+2/3, -z+7/6'
 '-x, -y, -z'
 'y, -x+y, -z'
 '-y, -x, z-1/2'
 'x-y, x, -z'
 'x, x-y, z-1/2'
 '-x+y, y, z-1/2'
 '-x+2/3, -y+1/3, -z+1/3'
 'y+2/3, -x+y+1/3, -z+1/3'
 '-y+2/3, -x+1/3, z-1/6'
 'x-y+2/3, x+1/3, -z+1/3'
 'x+2/3, x-y+1/3, z-1/6'
 '-x+y+2/3, y+1/3, z-1/6'
 '-x+1/3, -y+2/3, -z+2/3'
 'y+1/3, -x+y+2/3, -z+2/3'
 '-y+1/3, -x+2/3, z+1/6'
 'x-y+1/3, x+2/3, -z+2/3'
 'x+1/3, x-y+2/3, z+1/6'
 '-x+y+1/3, y+2/3, z+1/6'
 
_cell_length_a                    13.0933(11)
_cell_length_b                    13.0933(11)
_cell_length_c                    102.682(9)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 120.00
_cell_volume                      15245(2)
_cell_formula_units_Z             18
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     3613
_cell_measurement_theta_min       2.38
_cell_measurement_theta_max       25.85
 
_exptl_crystal_description        tablet
_exptl_crystal_colour             pale-yellow
_exptl_crystal_size_max           0.08
_exptl_crystal_size_mid           0.08
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.763
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              11398
_exptl_absorpt_coefficient_mu     18.524
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.638
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_process_details    SADABS
 
_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   'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method        'omega scan'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             19521
_diffrn_reflns_av_R_equivalents   0.0752
_diffrn_reflns_av_sigmaI/netI     0.0433
_diffrn_reflns_limit_h_min        -19
_diffrn_reflns_limit_h_max        19
_diffrn_reflns_limit_k_min        -19
_diffrn_reflns_limit_k_max        19
_diffrn_reflns_limit_l_min        -147
_diffrn_reflns_limit_l_max        147
_diffrn_reflns_theta_min          1.19
_diffrn_reflns_theta_max          31.25
_reflns_number_total              1851
_reflns_number_gt                 1289
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_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^)+(0.0496P)^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     none
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          1851
_refine_ls_number_parameters      110
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0619
_refine_ls_R_factor_gt            0.0345
_refine_ls_wR_factor_ref          0.0993
_refine_ls_wR_factor_gt           0.0933
_refine_ls_goodness_of_fit_ref    1.070
_refine_ls_restrained_S_all       1.070
_refine_ls_shift/su_max           0.049
_refine_ls_shift/su_mean          0.033
 
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_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Bi1 Bi 0.66697(3) 0.66628(4) 0.061525(1) 0.03218(2) Uani 1 1 d . . .
Bi2 Bi 0.3333 0.6667 0.001711(1) 0.02618(4) Uani 1 3 d S . .
Bi3 Bi 0.3333 0.6667 0.1667 0.03851(8) Uani 1 6 d S . .
Cl1 Cl 0.42424(5) 0.53716(5) 0.061762(6) 0.03377(18) Uani 1 1 d . . .
Cl2 Cl 0.90924(5) 0.77942(5) 0.061746(6) 0.03326(19) Uani 1 1 d . . .
Cl3 Cl 0.66682(5) 0.50816(5) 0.044966(7) 0.03919(18) Uani 1 1 d . . .
Cl4 Cl 0.66707(6) 0.79390(6) 0.042206(7) 0.0623(2) Uani 0.7784(15) 1 d P . .
Br4 Br 0.66707(6) 0.79390(6) 0.042206(7) 0.0623(2) Uani 0.2216(15) 1 d P . .
Cl5 Cl 0.6667 0.51733(7) 0.0833 0.0310(2) Uani 1 2 d S . .
Cl6 Cl 0.6667 0.81028(6) 0.0833 0.0573(2) Uani 0.686(2) 2 d SP . .
Br6 Br 0.6667 0.81028(6) 0.0833 0.0573(2) Uani 0.314(2) 2 d SP . .
Cl7 Cl 0.37243(6) 0.51729(5) 0.015372(10) 0.0865(3) Uani 0.6667(16) 1 d P . .
Br7 Br 0.37243(6) 0.51729(5) 0.015372(10) 0.0865(3) Uani 0.3333(16) 1 d P . .
Cl8 Cl 0.34075(6) 0.83637(6) -0.015537(8) 0.0458(2) Uani 1 1 d . . .
Cl9 Cl 0.19199(7) 0.47653(7) 0.181760(14) 0.0843(4) Uani 1 1 d . . .
N1 N 0.3378(4) 0.9918(3) 0.011783(15) 0.0460(4) Uiso 1 1 d . . .
N2 N 0.6667 1.04908(13) 0.0833 0.0426(4) Uiso 0.643(3) 2 d SP . .
K2 K 0.6667 1.04908(13) 0.0833 0.0426(4) Uiso 0.357(3) 2 d SP . .
N3 N 0.33370(11) 0.95776(9) -0.038254(13) 0.0395(3) Uiso 0.738(2) 1 d P . .
K3 K 0.33370(11) 0.95776(9) -0.038254(13) 0.0395(3) Uiso 0.262(2) 1 d P . .
N4 N 0.3333 0.6667 0.04085(3) 0.0735(7) Uiso 0.508(5) 3 d SP . .
K4 K 0.3333 0.6667 0.04085(3) 0.0735(7) Uiso 0.492(5) 3 d SP . .
N5 N 0.3333 0.6667 0.08236(6) 0.0252(6) Uiso 1 3 d S . .
N6 N 0.0000 0.0000 0.04037(4) 0.0461(11) Uiso 1 3 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
Bi1 0.01539(2) 0.04562(3) 0.02683(2) -0.00098(19) -0.00050(12) 0.00872(3)
Bi2 0.03031(3) 0.03031(3) 0.01793(8) 0.000 0.000 0.01515(2)
Bi3 0.01684(6) 0.01684(6) 0.0818(2) 0.000 0.000 0.00842(3)
Cl1 0.02675(19) 0.0458(2) 0.0356(3) 0.0010(2) 0.0014(2) 0.02329(16)
Cl2 0.0270(2) 0.0286(2) 0.0325(3) -0.0019(2) -0.0014(2) 0.00514(18)
Cl3 0.01537(19) 0.0379(2) 0.0571(3) -0.0304(2) 0.0004(2) 0.00786(16)
Cl4 0.0869(3) 0.0590(3) 0.0483(3) 0.0141(3) 0.0003(3) 0.0421(2)
Br4 0.0869(3) 0.0590(3) 0.0483(3) 0.0141(3) 0.0003(3) 0.0421(2)
Cl5 0.0219(4) 0.0304(3) 0.0378(4) -0.00044(17) -0.0009(3) 0.01096(19)
Cl6 0.0930(7) 0.0482(3) 0.0456(4) -0.0015(2) -0.0031(5) 0.0465(3)
Br6 0.0930(7) 0.0482(3) 0.0456(4) -0.0015(2) -0.0031(5) 0.0465(3)
Cl7 0.0721(3) 0.0598(2) 0.1442(7) 0.0151(4) 0.0129(4) 0.04556(17)
Br7 0.0721(3) 0.0598(2) 0.1442(7) 0.0151(4) 0.0129(4) 0.04556(17)
Cl8 0.0466(2) 0.0532(3) 0.0509(4) -0.0028(3) -0.0084(3) 0.03500(18)
Cl9 0.0406(3) 0.0367(3) 0.1736(11) -0.0044(5) 0.0183(5) 0.0177(2)
 
_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
Bi1 Cl4 2.5932(8) . ?
Bi1 Cl3 2.6782(9) . ?
Bi1 Cl2 2.7493(7) . ?
Bi1 Cl1 2.7542(6) . ?
Bi1 Cl6 2.9286(6) . ?
Bi1 Cl5 2.9682(7) . ?
Bi2 Br7 2.6563(9) 4_565 ?
Bi2 Br7 2.6563(9) 2_665 ?
Bi2 Cl7 2.6563(9) 4_565 ?
Bi2 Cl7 2.6563(9) 2_665 ?
Bi2 Cl7 2.6563(9) . ?
Bi2 Cl8 2.8049(9) . ?
Bi2 Cl8 2.8049(9) 2_665 ?
Bi2 Cl8 2.8049(9) 4_565 ?
Bi3 Cl9 2.7233(10) 28 ?
Bi3 Cl9 2.7233(10) 25_565 ?
Bi3 Cl9 2.7233(10) 26_455 ?
Bi3 Cl9 2.7234(10) 4_565 ?
Bi3 Cl9 2.7234(10) 2_665 ?
Bi3 Cl9 2.7234(10) . ?
Cl1 K2 3.2964(8) 15_444 ?
Cl1 K3 3.4115(14) 22_655 ?
Cl2 K2 3.2951(9) 2_765 ?
Cl2 K3 3.4136(16) 20 ?
Cl3 K3 3.3908(18) 22_655 ?
Cl3 K3 3.3925(12) 20 ?
Cl4 K3 3.2819(17) 19_675 ?
Cl5 Bi1 2.9680(7) 17_654 ?
Cl5 K2 3.2695(14) 15_444 ?
Cl5 K2 3.2695(13) 2_765 ?
Cl6 Bi1 2.9284(6) 17_654 ?
Cl7 K3 3.3781(15) 22_655 ?
Cl9 K3 3.4336(19) 17_544 ?
 
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
Cl4 Bi1 Cl3 90.69(2) . . ?
Cl4 Bi1 Cl2 91.74(2) . . ?
Cl3 Bi1 Cl2 88.65(2) . . ?
Cl4 Bi1 Cl1 91.77(2) . . ?
Cl3 Bi1 Cl1 88.65(2) . . ?
Cl2 Bi1 Cl1 175.59(3) . . ?
Cl4 Bi1 Cl6 99.78(3) . . ?
Cl3 Bi1 Cl6 169.53(2) . . ?
Cl2 Bi1 Cl6 91.111(16) . . ?
Cl1 Bi1 Cl6 90.908(18) . . ?
Cl4 Bi1 Cl5 179.07(3) . . ?
Cl3 Bi1 Cl5 88.38(3) . . ?
Cl2 Bi1 Cl5 88.277(18) . . ?
Cl1 Bi1 Cl5 88.166(16) . . ?
Cl6 Bi1 Cl5 81.151(19) . . ?
Br7 Bi2 Br7 94.69(3) 4_565 2_665 ?
Br7 Bi2 Cl7 0.00(4) 4_565 4_565 ?
Br7 Bi2 Cl7 94.69(3) 2_665 4_565 ?
Br7 Bi2 Cl7 94.69(3) 4_565 2_665 ?
Br7 Bi2 Cl7 0.00(5) 2_665 2_665 ?
Cl7 Bi2 Cl7 94.69(3) 4_565 2_665 ?
Br7 Bi2 Cl7 94.69(3) 4_565 . ?
Br7 Bi2 Cl7 94.69(3) 2_665 . ?
Cl7 Bi2 Cl7 94.69(3) 4_565 . ?
Cl7 Bi2 Cl7 94.69(3) 2_665 . ?
Br7 Bi2 Cl8 98.45(2) 4_565 . ?
Br7 Bi2 Cl8 83.09(2) 2_665 . ?
Cl7 Bi2 Cl8 98.45(2) 4_565 . ?
Cl7 Bi2 Cl8 83.09(2) 2_665 . ?
Cl7 Bi2 Cl8 166.81(2) . . ?
Br7 Bi2 Cl8 83.09(2) 4_565 2_665 ?
Br7 Bi2 Cl8 166.81(2) 2_665 2_665 ?
Cl7 Bi2 Cl8 83.09(2) 4_565 2_665 ?
Cl7 Bi2 Cl8 166.81(2) 2_665 2_665 ?
Cl7 Bi2 Cl8 98.45(2) . 2_665 ?
Cl8 Bi2 Cl8 84.37(3) . 2_665 ?
Br7 Bi2 Cl8 166.81(2) 4_565 4_565 ?
Br7 Bi2 Cl8 98.45(2) 2_665 4_565 ?
Cl7 Bi2 Cl8 166.81(2) 4_565 4_565 ?
Cl7 Bi2 Cl8 98.45(2) 2_665 4_565 ?
Cl7 Bi2 Cl8 83.09(2) . 4_565 ?
Cl8 Bi2 Cl8 84.37(3) . 4_565 ?
Cl8 Bi2 Cl8 84.37(3) 2_665 4_565 ?
Cl9 Bi3 Cl9 90.82(4) 28 25_565 ?
Cl9 Bi3 Cl9 90.82(4) 28 26_455 ?
Cl9 Bi3 Cl9 90.82(4) 25_565 26_455 ?
Cl9 Bi3 Cl9 179.996(1) 28 4_565 ?
Cl9 Bi3 Cl9 89.18(4) 25_565 4_565 ?
Cl9 Bi3 Cl9 89.18(4) 26_455 4_565 ?
Cl9 Bi3 Cl9 89.18(4) 28 2_665 ?
Cl9 Bi3 Cl9 89.18(4) 25_565 2_665 ?
Cl9 Bi3 Cl9 180.0 26_455 2_665 ?
Cl9 Bi3 Cl9 90.82(4) 4_565 2_665 ?
Cl9 Bi3 Cl9 89.18(4) 28 . ?
Cl9 Bi3 Cl9 180.00(4) 25_565 . ?
Cl9 Bi3 Cl9 89.18(4) 26_455 . ?
Cl9 Bi3 Cl9 90.82(4) 4_565 . ?
Cl9 Bi3 Cl9 90.82(4) 2_665 . ?
Bi1 Cl1 K2 100.17(3) . 15_444 ?
Bi1 Cl1 K3 100.34(3) . 22_655 ?
K2 Cl1 K3 87.26(3) 15_444 22_655 ?
Bi1 Cl2 K2 100.17(3) . 2_765 ?
Bi1 Cl2 K3 100.45(3) . 20 ?
K2 Cl2 K3 87.26(3) 2_765 20 ?
Bi1 Cl3 K3 102.49(3) . 22_655 ?
Bi1 Cl3 K3 102.51(3) . 20 ?
K3 Cl3 K3 153.10(5) 22_655 20 ?
Bi1 Cl4 K3 137.20(4) . 19_675 ?
Bi1 Cl5 Bi1 97.95(3) 17_654 . ?
Bi1 Cl5 K2 96.259(17) 17_654 15_444 ?
Bi1 Cl5 K2 96.381(16) . 15_444 ?
Bi1 Cl5 K2 96.384(16) 17_654 2_765 ?
Bi1 Cl5 K2 96.253(16) . 2_765 ?
K2 Cl5 K2 160.69(5) 15_444 2_765 ?
Bi1 Cl6 Bi1 99.74(3) 17_654 . ?
Bi2 Cl7 K3 165.34(4) . 22_655 ?
Bi3 Cl9 K3 164.63(5) . 17_544 ?
 
_diffrn_measured_fraction_theta_max    0.334
_diffrn_reflns_theta_full              31.25
_diffrn_measured_fraction_theta_full   0.334
_refine_diff_density_max    1.550
_refine_diff_density_min   -1.144
_refine_diff_density_rms    0.203