#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:07:45 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224190 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/97/7049734.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_7049734
loop_
_publ_author_name
'Ritter, Christian'
'Ringler, Benjamin'
'Dankert, Fabian'
'Conrad, Matthias'
'Kraus, Florian'
'von Hänisch, Carsten'
_publ_section_title
;
 Synthesis and crystal structures of novel tertiary butyl substituted
 (pseudo-)halogen bismuthanes.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5253
_journal_page_last               5262
_journal_paper_doi               10.1039/c9dt00408d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C8 H18 Bi N3'
_chemical_formula_sum            'C8 H18 Bi N3'
_chemical_formula_weight         365.23
_chemical_name_systematic        'Di tert butyl azidobismuthane'
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-23 deposited with the CCDC.    2019-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4387(16)
_cell_length_b                   11.4387(16)
_cell_length_c                   17.818(4)
_cell_measurement_reflns_used    6184
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.983
_cell_measurement_theta_min      2.116
_cell_volume                     2331.4(7)
_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(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6184
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.983
_diffrn_reflns_theta_min         2.116
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.085
_exptl_absorpt_correction_T_max  0.7681
_exptl_absorpt_correction_T_min  0.2233
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   'STOE X-Area, LANA'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_size_rad          0.1
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 438 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(12)
_refine_ls_extinction_coef       0.00079(8)
_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   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         1137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0167
_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)+(0.0208P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0360
_refine_ls_wR_factor_ref         0.0363
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                1065
_reflns_number_total             1137
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00408d1.cif
_cod_data_source_block           tBu2BiN3
_cod_depositor_comments
'Adding full bibliography for 7049733--7049739.cif.'
_cod_original_cell_volume        2331.4(8)
_cod_database_code               7049734
_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_max   0.211
_shelx_estimated_absorpt_t_min   0.152
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.86(2)
 0.14(2)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3.a Idealised Me refined as rotating group:
 C003(H00A,H00B,H00C), C004(H00D,H00E,H00F), C005(H00G,H00H,H00I)
;
_shelx_res_file
;
TITL pcr079a_a.res in I-42d
    pcr_079a.res
    created by SHELXL-2018/3 at 15:30:58 on 28-Jun-2018
REM Old TITL C:\Frames\PCR079a\PCR079a in I-42d
REM SHELXT solution in I-42d
REM R1 0.042, Rweak 0.011, Alpha 0.008, Orientation as input
REM Flack x = 0.181 ( 0.009 ) from Parsons' quotients
REM Formula found by SHELXT: C7 N4 Bi
CELL 0.71073 11.4387 11.4387 17.8184 90 90 90
ZERR 8 0.0016 0.0016 0.0036 0 0 0
LATT -2
SYMM -X,-Y,+Z
SYMM +Y,-X,-Z
SYMM -Y,+X,-Z
SYMM 0.5-X,+Y,0.75-Z
SYMM 0.5+X,-Y,0.75-Z
SYMM 0.5-Y,-X,0.75+Z
SYMM 0.5+Y,+X,0.75+Z
SFAC C H Bi N
UNIT 64 144 8 24

L.S. 4
PLAN  20
SIZE 0.15 0.15 0.2
TEMP -173(2)
BOND $H
list 4
fmap 2
acta
TWIN 0 1 0 -1 0 0 0 0 1 2
OMIT 0 52
OMIT 3 14 1
REM <olex2.extras>
REM <HklSrc "%.\\PCR_079a_01.hkl">
REM </olex2.extras>

WGHT    0.020800
EXTI    0.000785
BASF   0.14084
FVAR       0.21650
BI01  3    0.250000    0.403379    0.375000    10.50000    0.01438    0.01158 =
         0.01952    0.00000   -0.00057    0.00000
N002  4    0.458272    0.406507    0.418048    11.00000    0.02269    0.01971 =
         0.03324    0.00040    0.00210   -0.00965
C003  1    0.204985    0.232947    0.237948    11.00000    0.02007    0.02511 =
         0.03022   -0.00637   -0.00819   -0.00128
AFIX 137
H00A  2    0.232098    0.185591    0.195548    11.00000   -1.50000
H00B  2    0.158703    0.298860    0.219193    11.00000   -1.50000
H00C  2    0.156578    0.184763    0.271151    11.00000   -1.50000
AFIX   0
C004  1    0.384096    0.357283    0.229553    11.00000    0.02488    0.02919 =
         0.02157    0.00146    0.01151   -0.00214
AFIX 137
H00D  2    0.449902    0.389481    0.258068    11.00000   -1.50000
H00E  2    0.335822    0.421378    0.210278    11.00000   -1.50000
H00F  2    0.413882    0.310841    0.187477    11.00000   -1.50000
AFIX   0
C005  1    0.382995    0.178695    0.311752    11.00000    0.01750    0.02027 =
         0.03045    0.00004   -0.00232    0.00282
AFIX 137
H00G  2    0.414684    0.133044    0.269893    11.00000   -1.50000
H00H  2    0.334115    0.128269    0.343254    11.00000   -1.50000
H00I  2    0.447471    0.210235    0.341781    11.00000   -1.50000
AFIX   0
N006  4    0.500000    0.500000    0.416259    10.50000    0.00813    0.02724 =
         0.01706    0.00000    0.00000    0.00010
C007  1    0.309628    0.278827    0.281232    11.00000    0.01068    0.02067 =
         0.02377    0.00565   -0.00206   -0.00257
HKLF 4




REM  pcr079a_a.res in I-42d
REM wR2 = 0.0363, GooF = S = 1.037, Restrained GooF = 1.037 for all data
REM R1 = 0.0167 for 1065 Fo > 4sig(Fo) and 0.0187 for all 1137 data
REM 61 parameters refined using 0 restraints

END

WGHT      0.0208      0.0000

REM Highest difference peak  0.421,  deepest hole -0.494,  1-sigma level  0.108
Q1    1   0.2210  0.2500  0.1250  10.50000  0.05    0.42
Q2    1   0.2050  0.3567  0.3749  11.00000  0.05    0.42
Q3    1   0.2500  0.0404  0.3750  10.50000  0.05    0.40
Q4    1   0.3967  0.4152  0.1619  11.00000  0.05    0.37
Q5    1   0.2408  0.4824  0.2296  11.00000  0.05    0.36
Q6    1   0.4088  0.3373  0.3733  11.00000  0.05    0.35
Q7    1   0.4961  0.1054  0.3799  11.00000  0.05    0.34
Q8    1   0.3573  0.2500  0.1250  10.50000  0.05    0.34
Q9    1   0.3082  0.4703  0.2928  11.00000  0.05    0.33
Q10   1   0.1565  0.4291  0.2231  11.00000  0.05    0.33
Q11   1   0.6017  0.3859  0.3790  11.00000  0.05    0.33
Q12   1   0.3407  0.4429  0.4502  11.00000  0.05    0.33
Q13   1   0.4610  0.2681  0.3734  11.00000  0.05    0.32
Q14   1   0.5390  0.3994  0.4990  11.00000  0.05    0.31
Q15   1   0.0743  0.2364  0.3264  11.00000  0.05    0.30
Q16   1   0.2634  0.4064  0.2707  11.00000  0.05    0.29
Q17   1   0.3396  0.3059  0.2385  11.00000  0.05    0.29
Q18   1   0.3549  0.2355  0.2874  11.00000  0.05    0.29
Q19   1   0.4939  0.3662  0.4162  11.00000  0.05    0.28
Q20   1   0.1954  0.3484  0.2243  11.00000  0.05    0.28
;
_shelx_res_checksum              32351
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'
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 0.250000 0.40338(3) 0.375000 0.01516(12) Uani 1 2 d S T P
N1 N 0.4583(5) 0.4065(6) 0.4180(3) 0.0252(12) Uani 1 1 d . . .
C2 C 0.2050(6) 0.2329(7) 0.2379(4) 0.0251(16) Uani 1 1 d . . .
H2A H 0.232098 0.185591 0.195548 0.038 Uiso 1 1 calc GR . .
H2B H 0.158703 0.298860 0.219193 0.038 Uiso 1 1 calc GR . .
H2C H 0.156578 0.184763 0.271151 0.038 Uiso 1 1 calc GR . .
C4 C 0.3841(7) 0.3573(7) 0.2296(4) 0.0252(16) Uani 1 1 d . . .
H4D H 0.449902 0.389481 0.258068 0.038 Uiso 1 1 calc GR . .
H4E H 0.335822 0.421378 0.210278 0.038 Uiso 1 1 calc GR . .
H4F H 0.413882 0.310841 0.187477 0.038 Uiso 1 1 calc GR . .
C3 C 0.3830(6) 0.1787(6) 0.3118(4) 0.0227(16) Uani 1 1 d . . .
H3G H 0.414684 0.133044 0.269893 0.034 Uiso 1 1 calc GR . .
H3H H 0.334115 0.128269 0.343254 0.034 Uiso 1 1 calc GR . .
H3I H 0.447471 0.210235 0.341781 0.034 Uiso 1 1 calc GR . .
N2 N 0.500000 0.500000 0.4163(5) 0.0175(17) Uani 1 2 d S T P
C1 C 0.3096(5) 0.2788(6) 0.2812(4) 0.0184(14) Uani 1 1 d . . .
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 0.01438(17) 0.01158(17) 0.01952(15) 0.000 -0.00057(15) 0.000
N1 0.023(3) 0.020(3) 0.033(3) 0.000(3) 0.002(3) -0.010(3)
C2 0.020(3) 0.025(4) 0.030(4) -0.006(3) -0.008(3) -0.001(3)
C4 0.025(4) 0.029(4) 0.022(3) 0.001(3) 0.012(3) -0.002(3)
C3 0.017(4) 0.020(3) 0.030(4) 0.000(3) -0.002(3) 0.003(3)
N2 0.008(4) 0.027(5) 0.017(4) 0.000 0.000 0.000(3)
C1 0.011(3) 0.021(4) 0.024(3) 0.006(3) -0.002(3) -0.003(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
N N 0.0061 0.0033 '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
N1 Bi1 N1 178.4(3) . 5
C1 Bi1 N1 93.9(2) . 5
C1 Bi1 N1 87.1(2) 5 5
C1 Bi1 N1 93.9(2) 5 .
C1 Bi1 N1 87.1(2) . .
C1 Bi1 C1 103.4(3) . 5
N2 N1 Bi1 113.1(4) . .
H2A C2 H2B 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H4D C4 H4E 109.5 . .
H4D C4 H4F 109.5 . .
H4E C4 H4F 109.5 . .
C1 C4 H4D 109.5 . .
C1 C4 H4E 109.5 . .
C1 C4 H4F 109.5 . .
H3G C3 H3H 109.5 . .
H3G C3 H3I 109.5 . .
H3H C3 H3I 109.5 . .
C1 C3 H3G 109.5 . .
C1 C3 H3H 109.5 . .
C1 C3 H3I 109.5 . .
N1 N2 N1 176.9(10) . 2_665
C2 C1 Bi1 110.5(4) . .
C2 C1 C4 109.5(6) . .
C2 C1 C3 110.9(6) . .
C4 C1 Bi1 103.7(5) . .
C3 C1 Bi1 111.8(5) . .
C3 C1 C4 110.3(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Bi1 N1 2.503(6) .
Bi1 N1 2.503(6) 5
Bi1 C1 2.299(7) .
Bi1 C1 2.299(7) 5
N1 N2 1.172(6) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C2 C1 1.518(9) .
C4 H4D 0.9800 .
C4 H4E 0.9800 .
C4 H4F 0.9800 .
C4 C1 1.542(9) .
C3 H3G 0.9800 .
C3 H3H 0.9800 .
C3 H3I 0.9800 .
C3 C1 1.521(9) .
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.86(2)
2 0.14(2)
