#------------------------------------------------------------------------------
#$Date: 2019-11-03 12:30:04 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221390 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/82/4128268.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_4128268
loop_
_publ_author_name
'Morad, Viktoriia'
'Shynkarenko, Yevhen'
'Yakunin, Sergii'
'Brumberg, Alexandra'
'Schaller, Richard D.'
'Kovalenko, Maksym V.'
_publ_section_title
;
 Disphenoidal Zero-Dimensional Lead, Tin, and Germanium Halides: Highly
 Emissive Singlet and Triplet Self-Trapped Excitons and X-ray
 Scintillation.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9764
_journal_page_last               9768
_journal_paper_doi               10.1021/jacs.9b02365
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'Br4 Pb, 2(C10 H22 N)'
_chemical_formula_sum            'C20 H44 Br4 N2 Pb'
_chemical_formula_weight         839.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 123.796(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3640(9)
_cell_length_b                   8.4235(2)
_cell_length_c                   18.8888(9)
_cell_measurement_reflns_used    13211
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.5670
_cell_measurement_theta_min      1.9810
_cell_volume                     2692.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28c (Rigaku OD, 2015)'
_computing_data_collection       'SMART v5.630 (Bruker, 2003)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28c (Rigaku OD, 2015)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Apex I'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω      2.18 182.00   0.30   10.05    --   28.00  73.93 -25.82  600
  2  ω      2.18 182.00   0.30   10.06    --   28.00  73.93  94.18  600
  3  ω      2.18 182.00   0.30   10.07    --   28.00  73.93-145.82  600
;
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type
'Bruker SMART Platform with an Apex I-detector'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0119800000
_diffrn_orient_matrix_UB_12      -0.0553896000
_diffrn_orient_matrix_UB_13      0.0333182000
_diffrn_orient_matrix_UB_21      -0.0355897000
_diffrn_orient_matrix_UB_22      -0.0428917000
_diffrn_orient_matrix_UB_23      -0.0263222000
_diffrn_orient_matrix_UB_31      0.0185756000
_diffrn_orient_matrix_UB_32      -0.0467177000
_diffrn_orient_matrix_UB_33      -0.0153862000
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_unetI/netI     0.0123
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14568
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.474
_diffrn_reflns_theta_min         2.362
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    12.211
_exptl_absorpt_correction_T_max  0.07156
_exptl_absorpt_correction_T_min  0.04269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28c (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_recrystallization_method
'crystallized from a dimethylformamide/diethylether mixture'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         4117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0213
_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)+(0.0254P)²+7.4614P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0501
_refine_ls_wR_factor_ref         0.0508
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3946
_reflns_number_total             4117
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b02365_si_002.cif
_cod_data_source_block           a
_cod_database_code               4128268
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C80H176B16N8Pb4
_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   0.205
_shelx_estimated_absorpt_t_min   0.205
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed U12: Pb1(0)
 Fixed U23: Pb1(0)
 Fixed Uiso: H1A(0.026) H1B(0.026) H2A(0.029) H2B(0.029) H3A(0.032) H3B(0.032)
 H4A(0.027) H4B(0.027) H5A(0.026) H5B(0.026) H6A(0.024) H6B(0.024) H7A(0.027)
 H7B(0.027) H8A(0.026) H8B(0.026) H9A(0.044) H9B(0.044) H9C(0.044) H10A(0.039)
 H10B(0.039) H10C(0.039)
 Fixed X: Pb1(0.5) H1A(0.059648) H1B(0.054412) H2A(0.028195) H2B(-0.034771)
 H3A(0.017629) H3B(0.031974) H4A(0.150231) H4B(0.148372) H5A(0.238805)
 H5B(0.173238) H6A(0.239779) H6B(0.156869) H7A(0.189038) H7B(0.102518)
 H8A(0.148662) H8B(0.236642) H9A(0.108105) H9B(0.172132) H9C(0.198416)
 H10A(0.185297) H10B(0.258751) H10C(0.189946)
 Fixed Y: H1A(0.966926) H1B(0.835767) H2A(0.637405) H2B(0.777741)
 H3A(0.689624) H3B(0.875461) H4A(0.768795) H4B(0.630779) H5A(0.824905)
 H5B(0.960759) H6A(0.646327) H6B(0.580344) H7A(0.678916) H7B(0.628682)
 H8A(0.370599) H8B(0.41992) H9A(0.411655) H9B(0.272697) H9C(0.444656)
 H10A(0.932527) H10B(0.922658) H10C(1.049439)
 Fixed Z: Pb1(0.75) H1A(0.576607) H1B(0.512356) H2A(0.57989) H2B(0.551669)
 H3A(0.694502) H3B(0.690609) H4A(0.803378) H4B(0.743934) H5A(0.762132)
 H5B(0.730221) H6A(0.663225) H6B(0.641054) H7A(0.518585) H7B(0.493199)
 H8A(0.54849) H8B(0.579152) H9A(0.403425) H9B(0.44871) H9C(0.437216)
 H10A(0.554276) H10B(0.651503) H10C(0.623716)
;
_olex2_exptl_crystal_mounting_method tip-mounted
_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 1.288
_oxdiff_exptl_absorpt_empirical_full_min 0.772
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Pb1 Pb 0.500000 0.78841(2) 0.750000 0.01899(4) Uani 1 2 d S T P
Br1 Br 0.58730(2) 0.79025(3) 0.66360(2) 0.02200(6) Uani 1 1 d . . .
Br2 Br 0.39055(2) 0.57918(3) 0.63434(2) 0.02443(6) Uani 1 1 d . . .
N1 N 0.15829(12) 0.8234(2) 0.63149(13) 0.0191(4) Uani 1 1 d . . .
C1 C 0.07051(14) 0.8543(3) 0.57171(15) 0.0214(4) Uani 1 1 d . . .
H1A H 0.059648 0.966926 0.576607 0.026 Uiso 1 1 calc R . .
H1B H 0.054412 0.835767 0.512356 0.026 Uiso 1 1 calc R . .
C2 C 0.02176(15) 0.7496(3) 0.59052(16) 0.0241(5) Uani 1 1 d . . .
H2A H 0.028195 0.637405 0.579890 0.029 Uiso 1 1 calc R . .
H2B H -0.034771 0.777741 0.551669 0.029 Uiso 1 1 calc R . .
C3 C 0.04648(16) 0.7680(4) 0.68253(18) 0.0270(5) Uani 1 1 d . . .
H3A H 0.017629 0.689624 0.694502 0.032 Uiso 1 1 calc R . .
H3B H 0.031974 0.875461 0.690609 0.032 Uiso 1 1 calc R . .
C4 C 0.13517(15) 0.7435(3) 0.74497(16) 0.0225(5) Uani 1 1 d . . .
H4A H 0.150231 0.768795 0.803378 0.027 Uiso 1 1 calc R . .
H4B H 0.148372 0.630779 0.743934 0.027 Uiso 1 1 calc R . .
C5 C 0.18178(15) 0.8481(3) 0.72250(15) 0.0218(4) Uani 1 1 d . . .
H5A H 0.238805 0.824905 0.762132 0.026 Uiso 1 1 calc R . .
H5B H 0.173238 0.960759 0.730221 0.026 Uiso 1 1 calc R . .
C7 C 0.18182(14) 0.6570(3) 0.62318(15) 0.0197(4) Uani 1 1 d . . .
H6A H 0.239779 0.646327 0.663225 0.024 Uiso 1 1 calc R . .
H6B H 0.156869 0.580344 0.641054 0.024 Uiso 1 1 calc R . .
C8 C 0.15978(15) 0.6115(3) 0.53504(15) 0.0227(5) Uani 1 1 d . . .
H7A H 0.189038 0.678916 0.518585 0.027 Uiso 1 1 calc R . .
H7B H 0.102518 0.628682 0.493199 0.027 Uiso 1 1 calc R . .
C9 C 0.18002(15) 0.4375(3) 0.53461(15) 0.0216(4) Uani 1 1 d . . .
H8A H 0.148662 0.370599 0.548490 0.026 Uiso 1 1 calc R . .
H8B H 0.236642 0.419920 0.579152 0.026 Uiso 1 1 calc R . .
C10 C 0.16316(17) 0.3871(4) 0.44824(18) 0.0291(5) Uani 1 1 d . . .
H9A H 0.108105 0.411655 0.403425 0.044 Uiso 1 1 calc GR . .
H9B H 0.172132 0.272697 0.448710 0.044 Uiso 1 1 calc GR . .
H9C H 0.198416 0.444656 0.437216 0.044 Uiso 1 1 calc GR . .
C6 C 0.20181(16) 0.9422(3) 0.61372(17) 0.0260(5) Uani 1 1 d . . .
H10A H 0.185297 0.932527 0.554276 0.039 Uiso 1 1 calc GR . .
H10B H 0.258751 0.922658 0.651503 0.039 Uiso 1 1 calc GR . .
H10C H 0.189946 1.049439 0.623716 0.039 Uiso 1 1 calc GR . .
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'
Br Br -0.2901 2.4595 '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'
Pb Pb -3.3944 10.1111 '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
Br1 Pb1 Br1 179.409(10) . 2_656
Br2 Pb1 Br1 92.005(8) . .
Br2 Pb1 Br1 88.377(8) 2_656 .
Br2 Pb1 Br1 88.378(8) . 2_656
Br2 Pb1 Br1 92.005(8) 2_656 2_656
Br2 Pb1 Br2 99.429(13) . 2_656
C1 N1 C5 108.55(19) . .
C1 N1 C7 113.03(18) . .
C7 N1 C5 108.92(18) . .
C6 N1 C1 108.63(19) . .
C6 N1 C5 108.04(19) . .
C6 N1 C7 109.5(2) . .
C2 C1 N1 112.5(2) . .
C1 C2 C3 111.4(2) . .
C2 C3 C4 111.5(2) . .
C5 C4 C3 111.1(2) . .
C4 C5 N1 112.6(2) . .
C8 C7 N1 115.49(19) . .
C7 C8 C9 109.5(2) . .
C8 C9 C10 111.8(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 Br1 3.0087(3) .
Pb1 Br1 3.0088(3) 2_656
Pb1 Br2 2.7258(3) .
Pb1 Br2 2.7258(3) 2_656
N1 C1 1.514(3) .
N1 C5 1.521(3) .
N1 C7 1.518(3) .
N1 C6 1.493(3) .
C1 C2 1.511(4) .
C2 C3 1.525(4) .
C3 C4 1.525(4) .
C4 C5 1.518(4) .
C7 C8 1.513(3) .
C8 C9 1.524(4) .
C9 C10 1.528(3) .
