Bi4O4Cu1.7Se2.7Cl0.3: Intergrowth of BiOCuSe and Bi2O2Se Stabilized by the Addition of a Third Anion.
Gibson, Quinn D.; Dyer, Matthew S.; Whitehead, George F. S.; Alaria, Jonathan; Pitcher, Michael J.; Edwards, Holly J.; Claridge, John B.; Zanella, Marco; Dawson, Karl; Manning, Troy D.; Dhanak, Vin R.; Rosseinsky, Matthew J.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b06168

data_4126648
_publ_section_title
;
 Bi4O4Cu1.7Se2.7Cl0.3: Intergrowth of BiOCuSe and Bi2O2Se Stabilized by
 the Addition of a Third Anion.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b06168
_journal_year                    2017
_chemical_formula_moiety         '2(Bi4 Cu1.73 O4 Se2), 1.35(Se), 0.65(Cl)'
_chemical_formula_sum            'Bi8 Cl0.64 Cu3.46 O8 Se5.36'
_chemical_formula_weight         2465.17
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_Hall           '-I 4 2'
_space_group_name_H-M_alt        'I 4/m m m'
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_primary     dual
_audit_creation_date             2016-12-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   3.89790(10)
_cell_length_b                   3.89790(10)
_cell_length_c                   29.8291(13)
_cell_measurement_reflns_used    1872
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.9680
_cell_measurement_theta_min      2.7160
_cell_volume                     453.21(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9947
_diffrn_measured_fraction_theta_max 0.9961
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -110.00  15.00   1.00    1.00    --  -20.00 -68.00   0.00  125
  2  \w   -110.00  15.00   1.00    1.00    --  -20.00 -68.00 120.00  125
  3  \w   -110.00  15.00   1.00    1.00    --  -20.00 -68.00 240.00  125
  4  \w   -110.00  15.00   1.00    1.00    --  -20.00 -30.00  90.00  125
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0708588000
_diffrn_orient_matrix_UB_12      0.0985147000
_diffrn_orient_matrix_UB_13      -0.0177164000
_diffrn_orient_matrix_UB_21      -0.0698422000
_diffrn_orient_matrix_UB_22      0.1164314000
_diffrn_orient_matrix_UB_23      0.0158303000
_diffrn_orient_matrix_UB_31      0.1523370000
_diffrn_orient_matrix_UB_32      0.0992956000
_diffrn_orient_matrix_UB_33      -0.0009894000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            3394
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.029
_diffrn_reflns_theta_min         2.731
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    92.178
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    9.032
_exptl_crystal_description       block
_exptl_crystal_F_000             1021
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.736
_refine_diff_density_min         -2.163
_refine_diff_density_rms         0.490
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     20
_refine_ls_number_reflns         258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+3.0443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                234
_reflns_number_total             258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b06168_si_002.cif
_cod_data_source_block           c9_qdg_5_2_100k
_cod_database_code               4126648
_chemical_oxdiff_formula         Bi4Cl0.3Cu1.7O4Se2.7
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Shared sites
{Se04, Cl}
2. Uiso/Uaniso restraints and constraints
Uanis(Se04) = Uanis(Cl)
3. Others
 Sof(Cl)=0.0625*(1-FVAR(2))
 Sof(Se04)=0.0625*FVAR(2)
;
_shelx_res_checksum              84370
_shelx_hkl_checksum              22311
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.519
_oxdiff_exptl_absorpt_empirical_full_min 0.618