#------------------------------------------------------------------------------
#$Date: 2019-05-01 01:12:56 +0300 (Wed, 01 May 2019) $
#$Revision: 214853 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/33/7123352.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_7123352
loop_
_publ_author_name
'Wei, Zheng'
'Dubceac, Cristina'
'Petrukhina, Marina A.'
'Dikarev, Evgeny V.'
_publ_section_title
;
 From a volatile molecular precursor to twin-free single crystals of
 bismuth
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02820J
_journal_year                    2019
_chemical_formula_moiety         Bi
_chemical_formula_sum            Bi
_chemical_formula_weight         208.98
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m'
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-09-13 deposited with the CCDC.    2019-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   4.5481(5)
_cell_length_b                   4.5481(5)
_cell_length_c                   11.8600(12)
_cell_measurement_reflns_used    3769
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      36.26
_cell_measurement_theta_min      5.16
_cell_volume                     212.46(4)
_computing_cell_refinement       'SAINT V.8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'APEX3 v.2017.3-0 (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V.8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'Xshell v.6.3.1 (Bruker AXS Inc., 2016)'
_computing_publication_material  'APEX3 v.2017.3-0 (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4485
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.327
_diffrn_reflns_theta_min         5.157
_exptl_absorpt_coefficient_mu    123.694
_exptl_absorpt_correction_T_max  0.0504
_exptl_absorpt_correction_T_min  0.0051
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker, 2016/2) was 
used for absorption correction. 
Krause, L., Herbst-Irmer, R., 
Sheldrick G.M. & Stalke D.,
J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            'metallic silver'
_exptl_crystal_density_diffrn    9.800
_exptl_crystal_description       block
_exptl_crystal_F_000             498
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.410
_refine_diff_density_min         -1.430
_refine_diff_density_rms         0.349
_refine_ls_extinction_coef       0.0081(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.429
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     5
_refine_ls_number_reflns         150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.429
_refine_ls_R_factor_all          0.0122
_refine_ls_R_factor_gt           0.0120
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0124P)²+0.6610P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0286
_refine_ls_wR_factor_ref         0.0287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                148
_reflns_number_total             150
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc02820j2.cif
_cod_data_source_block           300K
_cod_original_cell_volume        212.46(5)
_cod_database_code               7123352
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.025
_shelx_estimated_absorpt_t_max   0.049
_shelx_res_file
;
TITL final_a_a.res in R-3m
    final_a_a.res
    created by SHELXL-2018/3 at 09:57:01 on 18-May-2018
REM Old TITL final_a in R3m

REM SHELXT solution in R-3m
REM R1 0.047,  Rweak 0.021,  Alpha 0.001,  Orientation as input
REM Formula found by SHELXT:  Bi

CELL  0.71073   4.5481   4.5481  11.8600   90.000   90.000  120.000
ZERR    6.000   0.0005   0.0005   0.0012    0.000    0.000    0.000
LATT  3
SYMM -Y, X-Y, Z
SYMM -X+Y, -X, Z
SYMM Y, X, -Z
SYMM X-Y, -Y, -Z
SYMM -X, -X+Y, -Z
SFAC BI
UNIT 6
TEMP 26.850
SIZE 0.061 0.108 0.115
L.S. 40
BOND $H
ACTA
LIST 4
FMAP 2
PLAN 20
OMIT -1 1 1
WGHT    0.012400    0.661000
EXTI    0.008106
FVAR       0.29900
BI1   1    0.666667    0.333333    0.567242    10.16667    0.01993    0.01993 =
         0.01684    0.00000    0.00000    0.00996
HKLF 4




REM  final_a_a.res in R-3m
REM wR2 = 0.0287, GooF = S = 1.429, Restrained GooF = 1.429 for all data
REM R1 = 0.0120 for 148 Fo > 4sig(Fo) and 0.0122 for all 150 data
REM 5 parameters refined using 0 restraints

END

WGHT      0.0123      0.6682

REM Highest difference peak  1.410,  deepest hole -1.430,  1-sigma level  0.349
Q1    1   0.5703  0.1405  0.5693  10.50000  0.05    1.41
Q2    1   0.7565  0.2435  0.5657  10.50000  0.05    1.33
Q3    1   0.8600  0.7201  0.4269  10.50000  0.05    0.57
Q4    1   0.6667  0.3333  0.4390  10.16667  0.05    0.52
Q5    1   0.9330  0.2278  0.5784  11.00000  0.05    0.48
Q6    1   0.4754 -0.0491  0.5582  10.50000  0.05    0.38
Q7    1   0.7290  0.4579  0.6564  10.50000  0.05    0.36
Q8    1   0.8624  0.1376  0.6426  10.50000  0.05    0.30
Q9    1   0.5157  0.4843  0.6857  10.50000  0.05    0.13
Q10   1   0.1751  0.0876  0.4600  10.50000  0.05    0.11
Q11   1   0.9235  0.0765  0.5853  10.50000  0.05    0.11
;
_shelx_res_checksum              9243
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Bi1 Bi 0.666667 0.333333 0.56724(2) 0.01890(12) Uani 1 6 d S T P
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 0.01993(13) 0.01993(13) 0.01684(15) 0.000 0.000 0.00996(6)
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'
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
Bi1 Bi1 Bi1 95.493(11) 19_666 19_656
Bi1 Bi1 Bi1 95.493(11) 19_666 19_766
Bi1 Bi1 Bi1 95.492(11) 19_656 19_766
Bi1 Bi1 Bi1 91.660(6) 19_666 25_666
Bi1 Bi1 Bi1 169.348(13) 19_656 25_666
Bi1 Bi1 Bi1 91.660(6) 19_766 25_666
Bi1 Bi1 Bi1 169.348(13) 19_666 25_656
Bi1 Bi1 Bi1 91.659(7) 19_656 25_656
Bi1 Bi1 Bi1 91.659(7) 19_766 25_656
Bi1 Bi1 Bi1 80.228(11) 25_666 25_656
Bi1 Bi1 Bi1 91.660(6) 19_666 25_556
Bi1 Bi1 Bi1 91.660(6) 19_656 25_556
Bi1 Bi1 Bi1 169.348(13) 19_766 25_556
Bi1 Bi1 Bi1 80.228(11) 25_666 25_556
Bi1 Bi1 Bi1 80.228(11) 25_656 25_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Bi1 Bi1 3.0723(4) 19_666
Bi1 Bi1 3.0723(4) 19_656
Bi1 Bi1 3.0723(4) 19_766
Bi1 Bi1 3.5294(4) 25_666
Bi1 Bi1 3.5294(4) 25_656
Bi1 Bi1 3.5294(4) 25_556
