#------------------------------------------------------------------------------
#$Date: 2016-03-22 13:56:23 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178982 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/05/4120555.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_4120555
loop_
_publ_author_name
'Dohner, Emma R.'
'Hoke, Eric T.'
'Karunadasa, Hemamala I.'
_publ_section_title
;
 Self-assembly of broadband white-light emitters.
;
_journal_issue                   5
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1718
_journal_page_last               1721
_journal_paper_doi               10.1021/ja411045r
_journal_volume                  136
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_formula_moiety         'Br4 Pb, C3 H12 N2'
_chemical_formula_sum            'C3 H12 Br4 N2 Pb'
_chemical_formula_weight         602.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             2013-09-16
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.04.25 svn.r2679, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.0761(3)
_cell_length_b                   8.3926(5)
_cell_length_c                   23.7433(16)
_cell_measurement_reflns_used    8524
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.3528
_cell_measurement_theta_min      2.5747
_cell_volume                     1210.77(12)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.9911
_diffrn_measured_fraction_theta_max 0.9911
_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  0.0915
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            17740
_diffrn_reflns_theta_full        25.0270
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    27.086
_exptl_absorpt_correction_T_max  0.7734
_exptl_absorpt_correction_T_min  0.3445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS Inc.)'
_exptl_crystal_density_diffrn    3.3076
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.8787
_refine_diff_density_min         -1.8210
_refine_diff_density_rms         0.4601
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.54(2)
_refine_ls_d_res_high            0.8400
_refine_ls_d_res_low             7.9128
_refine_ls_goodness_of_fit_ref   1.0360
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    19
_refine_ls_number_parameters     81
_refine_ls_number_reflns         2125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0360
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0300P)²+3.8664P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.995
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              9
_reflns_limit_k_min              -9
_reflns_limit_l_max              28
_reflns_limit_l_min              -27
_reflns_number_gt                1789
_reflns_number_total             2125
_reflns_threshold_expression     I>=2u(I)
_iucr_refine_instructions_details
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C4) = Uanis(N2)
Uanis(C4) = Uanis(C3)
4.a Secondary CH2 refined with riding coordinates:
 N2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b)
4.b Idealised Me refined as rotating group:
 N1(H1a,H1b,H1c), C5(H5a,H5b,H5c)

;
_cod_data_source_file            ja411045r_si_002.cif
_cod_data_source_block           ds1
_cod_database_code               4120555
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x+1/2,-y+1/2,-z
3 -x,y+1/2,-z+1/2
4 -x+1/2,-y,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_refinement_flags_posn
_atom_site_refinement_flags_adp
Pb1 Pb 0.51417(10) 0.68169(5) 0.663352(17) 0.01251(13) Uani 1.000000 . U
Br2 Br 1.0332(2) 0.67350(13) 0.64595(5) 0.0165(3) Uani 1.000000 . U
Br4 Br 0.5210(2) 0.85405(12) 0.55577(5) 0.0168(3) Uani 1.000000 . U
Br5 Br 0.5353(2) 0.37094(13) 0.59780(5) 0.0177(3) Uani 1.000000 . U
Br1 Br 0.5020(3) 0.98817(12) 0.72590(4) 0.0190(3) Uani 1.000000 . U
N1 N 1.0243(19) 0.9638(10) 0.5297(4) 0.018(2) Uani 1.000000 . U
C5 C 1.000(3) 1.2648(12) 0.7086(4) 0.020(3) Uani 1.000000 . U
C3 C 1.014(3) 1.1098(11) 0.6207(4) 0.0153(16) Uani 1.000000 . U
C4 C 1.034(2) 1.1242(12) 0.5573(4) 0.0153(16) Uani 1.000000 . U
N2 N 1.0371(19) 1.2679(10) 0.6465(4) 0.0153(16) Uani 1.000000 . U
H1a H 1.048(13) 0.9746(15) 0.4920(6) 0.021(3) Uiso 1.000000 GR .
H1b H 1.130(9) 0.899(3) 0.545(2) 0.021(3) Uiso 1.000000 GR .
H1c H 0.889(5) 0.920(4) 0.535(3) 0.021(3) Uiso 1.000000 GR .
H5a H 0.848(5) 1.234(9) 0.7164(4) 0.030(4) Uiso 1.000000 GR .
H5b H 1.101(10) 1.188(7) 0.7259(6) 0.030(4) Uiso 1.000000 GR .
H5c H 1.028(12) 1.371(3) 0.7242(6) 0.030(4) Uiso 1.000000 GR .
H3a H 0.870(3) 1.0636(11) 0.6307(4) 0.0183(19) Uiso 1.000000 R .
H3b H 1.131(3) 1.0381(11) 0.6352(4) 0.0183(19) Uiso 1.000000 R .
H4a H 1.175(2) 1.1766(12) 0.5476(4) 0.0183(19) Uiso 1.000000 R .
H4b H 0.913(2) 1.1915(12) 0.5428(4) 0.0183(19) Uiso 1.000000 R .
H2a H 0.9373(19) 1.3363(10) 0.6303(4) 0.0183(19) Uiso 1.000000 R .
H2b H 1.1759(19) 1.3065(10) 0.6393(4) 0.0183(19) Uiso 1.000000 R .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pb1 0.0143(2) 0.0086(2) 0.0146(2) -0.0003(3) -0.0002(3) -0.00052(16)
Br2 0.0178(7) 0.0104(5) 0.0213(6) -0.0006(6) -0.0009(6) 0.0014(5)
Br4 0.0171(7) 0.0154(6) 0.0180(6) -0.0005(7) -0.0013(7) 0.0017(4)
Br5 0.0234(8) 0.0118(6) 0.0178(6) 0.0000(6) 0.0010(6) -0.0017(5)
Br1 0.0217(7) 0.0141(6) 0.0213(6) -0.0010(8) 0.0017(8) -0.0052(4)
N1 0.009(6) 0.018(5) 0.026(6) -0.009(6) 0.008(6) -0.006(4)
C5 0.022(7) 0.018(6) 0.019(6) 0.009(8) 0.013(9) -0.000(5)
C3 0.022(4) 0.010(3) 0.014(3) 0.001(3) 0.006(4) -0.005(2)
C4 0.022(4) 0.010(3) 0.014(3) 0.001(3) 0.006(4) -0.005(2)
N2 0.022(4) 0.010(3) 0.014(3) 0.001(3) 0.006(4) -0.005(2)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_dispersion_source
Pb -3.20855 10.15388
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Br -0.28346 2.55990 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
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
Br4 Pb1 Br2 84.48(4) . 1_455
Br5 Pb1 Br2 87.14(4) . 1_455
Br5 Pb1 Br4 88.66(3) . .
Br1 Pb1 Br2 93.76(4) . 1_455
Br1 Pb1 Br2 94.32(4) 3_646 1_455
Br1 Pb1 Br4 90.50(3) . .
Br1 Pb1 Br4 177.60(4) 3_646 .
Br1 Pb1 Br5 178.71(5) . .
Br1 Pb1 Br5 89.20(3) 3_646 .
N2 C3 C4 109.7(8) . .
C3 C4 N1 111.1(8) . .
C3 N2 C5 112.6(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 Br2 2.9521(16) 1_455
Pb1 Br4 2.9358(12) .
Pb1 Br5 3.0398(12) .
Pb1 Br1 3.0922(11) 3_646
Pb1 Br1 2.9710(11) .
N1 C4 1.498(12) .
C5 N2 1.490(13) .
C3 C4 1.516(14) .
C3 N2 1.468(12) .
