#------------------------------------------------------------------------------
#$Date: 2019-11-04 17:50:13 +0200 (Mon, 04 Nov 2019) $
#$Revision: 223184 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/29/4002910.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4002910
loop_
_publ_author_name
'Zhao, Jing'
'Hao, Shiqiang'
'Islam, Saiful M.'
'Chen, Haijie'
'Tan, Gangjian'
'Ma, Shulan'
'Wolverton, Christopher'
'Kanatzidis, Mercouri G.'
_publ_section_title
;
 Six Quaternary Chalcogenides of the Pavonite Homologous Series with
 Ultralow Lattice Thermal Conductivity
;
_journal_issue                   9
_journal_name_full               'Chemistry of Materials'
_journal_page_first              3430
_journal_paper_doi               10.1021/acs.chemmater.9b00585
_journal_volume                  31
_journal_year                    2019
_chemical_formula_moiety         '0.5(Bi6.96 In1.03 Mn4.06 Se16)'
_chemical_formula_sum            'Bi3.48 In0.51 Mn2.03 Se8'
_chemical_formula_weight         1529.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-01-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 115.43
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.279
_cell_length_b                   4.066
_cell_length_c                   14.988
_cell_measurement_reflns_used    3791
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.44
_cell_measurement_theta_min      3.01
_cell_volume                     730.832
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1271
_diffrn_reflns_av_unetI/netI     0.0857
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2400
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    64.123
_exptl_crystal_density_diffrn    6.950
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1274
_refine_diff_density_max         4.543
_refine_diff_density_min         -3.012
_refine_diff_density_rms         0.698
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.827
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.827
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1230P)²+418.6491P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1804
_refine_ls_wR_factor_ref         0.1908
_reflns_number_gt                683
_reflns_number_total             743
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm9b00585_si_002.cif
_cod_data_source_block           jz1266i-jana
_cod_depositor_comments
'Adding full bibliography for 4002910--4002915.cif.'
_cod_original_cell_volume        730.9
_cod_database_code               4002910
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.858(6)
 0.142(6)
2. Shared sites
{In3, Mn3}
{Bi2, Mn2}
3. Uiso/Uaniso restraints and constraints
Uanis(In3) = Uanis(Mn3)
Uanis(Bi2) = Uanis(Mn2)
4. Others
 Fixed Sof: Bi1(0.47) Bi2(0.4) Mn2(0.13) In3(0.129) Mn3(0.128)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z'
5 '-x, -y, -z'
6 'x, -y, z'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z'
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_calc_flag
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Bi1 Bi 0.71762(16) 0.0000 0.36017(16) 0.0284(6) Uani 0.94 d 2 S T P
Bi2 Bi 0.84883(16) -1.5000 0.13000(14) 0.0227(6) Uani 0.80 d 2 S T P
Mn2 Mn 0.84883(16) -1.5000 0.13000(14) 0.0227(6) Uani 0.26 d 2 S T P
In3 In 1.0000 -1.0000 0.0000 0.0256(14) Uani 0.52 d 4 S T P
Mn3 Mn 1.0000 -1.0000 0.0000 0.0256(14) Uani 0.51 d 4 S T P
Mn4 Mn 1.0000 -0.5000 0.5000 0.034(3) Uani 1 d 4 S T P
Se1 Se 0.8854(4) 0.0000 0.5454(3) 0.0209(10) Uani 1 d 2 S T P
Se3 Se 0.8432(4) -0.5000 0.3234(4) 0.0250(11) Uani 1 d 2 S T P
Se4 Se 0.8411(4) -0.5000 -0.0626(4) 0.0230(10) Uani 1 d 2 S T P
Se5 Se 1.0067(4) -1.0000 0.1827(4) 0.0243(11) Uani 1 d 2 S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
Se1 Bi1 Se1 82.12(13) . 7_646
Se1 Bi1 Se1 82.12(13) . 7_656
Se1 Bi1 Se1 81.65(13) 7_646 7_656
Se1 Bi1 Se3 84.57(13) . .
Se1 Bi1 Se3 84.57(13) . 1_565
Se3 Bi1 Se1 165.83(16) . 7_656
Se3 Bi1 Se1 91.73(9) . 7_646
Se3 Bi1 Se1 165.83(16) 1_565 7_646
Se3 Bi1 Se1 91.73(9) 1_565 7_656
Se3 Bi1 Se3 91.85(16) 1_565 .
Se3 Bi2 Se4 87.66(13) 1_545 7_635
Se3 Bi2 Se4 87.66(13) 1_545 7_625
Se4 Bi2 Se3 176.82(15) 1_545 1_545
Se4 Bi2 Se4 83.48(12) 7_625 7_635
Se4 Bi2 Se4 89.97(12) 1_545 7_635
Se4 Bi2 Se4 89.97(12) 1_545 7_625
Se5 Bi2 Se3 93.15(13) 1_545 1_545
Se5 Bi2 Se3 93.15(13) . 1_545
Se5 Bi2 Se4 89.02(13) 1_545 1_545
Se5 Bi2 Se4 174.63(11) 1_545 7_635
Se5 Bi2 Se4 91.25(9) 1_545 7_625
Se5 Bi2 Se4 174.63(11) . 7_625
Se5 Bi2 Se4 89.02(13) . 1_545
Se5 Bi2 Se4 91.25(9) . 7_635
Se5 Bi2 Se5 94.00(15) . 1_545
Se4 In3 Se4 86.31(14) 1_545 5_735
Se4 In3 Se4 93.69(14) 1_545 .
Se4 In3 Se4 86.31(14) 5_745 .
Se4 In3 Se4 180.0(2) 5_745 1_545
Se4 In3 Se4 93.69(14) 5_745 5_735
Se4 In3 Se4 180.0 . 5_735
Se5 In3 Se4 88.17(12) . 5_745
Se5 In3 Se4 91.83(12) . 1_545
Se5 In3 Se4 88.17(12) . 5_735
Se5 In3 Se4 88.17(12) 5_735 .
Se5 In3 Se4 91.83(12) 5_735 5_735
Se5 In3 Se4 91.83(12) . .
Se5 In3 Se4 88.17(12) 5_735 1_545
Se5 In3 Se4 91.83(12) 5_735 5_745
Se5 In3 Se5 180.0 5_735 .
Se1 Mn4 Se1 86.57(13) 1_545 5_746
Se1 Mn4 Se1 93.43(13) 5_756 5_746
Se1 Mn4 Se1 180.0 5_756 1_545
Se1 Mn4 Se1 86.57(13) 5_756 .
Se1 Mn4 Se1 93.43(13) 1_545 .
Se1 Mn4 Se1 180.00(19) 5_746 .
Se3 Mn4 Se1 91.95(12) . 5_746
Se3 Mn4 Se1 88.05(12) 5_746 5_756
Se3 Mn4 Se1 88.05(12) . .
Se3 Mn4 Se1 91.95(12) 5_746 1_545
Se3 Mn4 Se1 91.95(12) . 5_756
Se3 Mn4 Se1 88.05(12) . 1_545
Se3 Mn4 Se1 88.05(12) 5_746 5_746
Se3 Mn4 Se1 91.95(12) 5_746 .
Se3 Mn4 Se3 180.0 5_746 .
Bi1 Se1 Bi1 81.65(13) 7_646 7_656
Bi1 Se1 Bi1 97.88(13) . 7_646
Bi1 Se1 Bi1 97.88(13) . 7_656
Bi1 Se1 Mn4 92.56(12) . 1_565
Bi1 Se1 Mn4 92.56(12) . .
Mn4 Se1 Bi1 168.22(18) 1_565 7_646
Mn4 Se1 Bi1 91.56(3) . 7_646
Mn4 Se1 Bi1 91.56(3) 1_565 7_656
Mn4 Se1 Bi1 168.22(18) . 7_656
Mn4 Se1 Mn4 93.43(13) 1_565 .
Bi1 Se3 Bi1 91.85(16) 1_545 .
Bi1 Se3 Bi2 117.38(13) . 1_565
Bi1 Se3 Bi2 117.38(13) 1_545 1_565
Bi1 Se3 Mn2 117.38(13) 1_545 1_565
Bi1 Se3 Mn2 117.38(13) . 1_565
Mn2 Se3 Bi2 0.00(7) 1_565 1_565
Mn4 Se3 Bi1 94.82(13) . .
Mn4 Se3 Bi1 94.82(13) . 1_545
Mn4 Se3 Bi2 131.69(19) . 1_565
Mn4 Se3 Mn2 131.69(19) . 1_565
Bi2 Se4 Bi2 83.48(12) 7_625 7_635
Bi2 Se4 Bi2 90.03(12) 1_565 7_635
Bi2 Se4 Bi2 90.03(12) 1_565 7_625
Bi2 Se4 Mn2 0.00(8) 1_565 1_565
Mn2 Se4 Bi2 90.03(12) 1_565 7_635
Mn2 Se4 Bi2 90.03(12) 1_565 7_625
In3 Se4 Bi2 91.38(3) . 7_625
In3 Se4 Bi2 174.51(14) . 7_635
In3 Se4 Bi2 174.51(14) 1_565 7_625
In3 Se4 Bi2 88.05(12) . 1_565
In3 Se4 Bi2 88.05(12) 1_565 1_565
In3 Se4 Bi2 91.38(3) 1_565 7_635
In3 Se4 Mn2 88.05(12) 1_565 1_565
In3 Se4 Mn2 88.05(12) . 1_565
In3 Se4 In3 93.69(14) 1_565 .
Mn3 Se4 Bi2 91.38(3) 1_565 7_635
Mn3 Se4 Bi2 88.05(12) 1_565 1_565
Mn3 Se4 Bi2 174.51(14) 1_565 7_625
Mn3 Se4 Mn2 88.05(12) 1_565 1_565
Mn3 Se4 In3 0.0 1_565 1_565
Mn3 Se4 In3 93.69(14) 1_565 .
Bi2 Se5 Bi2 94.00(15) . 1_565
Bi2 Se5 Mn2 94.00(15) . 1_565
Mn2 Se5 Bi2 0.00(13) 1_565 1_565
In3 Se5 Bi2 91.11(13) . 1_565
In3 Se5 Bi2 91.11(13) . .
In3 Se5 Mn2 91.11(13) . 1_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Bi1 Se1 2.713(5) .
Bi1 Se1 3.110(4) 7_656
Bi1 Se1 3.110(4) 7_646
Bi1 Se3 2.830(4) .
Bi1 Se3 2.830(4) 1_565
Bi2 Se3 2.931(5) 1_545
Bi2 Se4 3.054(4) 7_625
Bi2 Se4 2.844(5) 1_545
Bi2 Se4 3.054(4) 7_635
Bi2 Se5 2.780(3) .
Bi2 Se5 2.780(3) 1_545
In3 Se4 2.787(3) 5_735
In3 Se4 2.787(3) 5_745
In3 Se4 2.787(3) 1_545
In3 Se4 2.787(3) .
In3 Se5 2.702(5) .
In3 Se5 2.702(5) 5_735
Mn4 Se1 2.793(3) 5_746
Mn4 Se1 2.793(3) .
Mn4 Se1 2.793(3) 1_545
Mn4 Se1 2.793(3) 5_756
Mn4 Se3 2.571(5) 5_746
Mn4 Se3 2.571(5) .
Se1 Bi1 3.110(4) 7_656
Se1 Bi1 3.110(4) 7_646
Se1 Mn4 2.793(3) 1_565
Se3 Bi1 2.830(4) 1_545
Se3 Bi2 2.931(5) 1_565
Se3 Mn2 2.931(5) 1_565
Se4 Bi2 3.054(4) 7_625
Se4 Bi2 3.054(4) 7_635
Se4 Bi2 2.844(5) 1_565
Se4 Mn2 2.844(5) 1_565
Se4 In3 2.787(3) 1_565
Se4 Mn3 2.787(3) 1_565
Se5 Bi2 2.780(3) 1_565
Se5 Mn2 2.780(3) 1_565
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.858(6)
2 0.142(6)
