#------------------------------------------------------------------------------
#$Date: 2020-05-22 01:21:03 +0300 (Fri, 22 May 2020) $
#$Revision: 252250 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/35/4003556.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_4003556
loop_
_publ_author_name
'Febriansyah, Benny'
'Neo, Chong Shern Daniel'
'Giovanni, David'
'Srivastava, Shivani'
'Lekina, Yulia'
'Koh, Teck Ming'
'Li, Yongxin'
'Shen, Ze Xiang'
'Asta, Mark'
'Sum, Tze Chien'
'Mathews, Nripan'
'England, Jason'
_publ_section_title
;
 Targeted Synthesis of Trimeric Organic--Bromoplumbate Hybrids That
 Display Intrinsic, Highly Stokes-Shifted, Broadband Emission
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.9b03925
_journal_year                    2020
_chemical_formula_sum            'C20 H32 Br5 N2 Pb1.5'
_chemical_formula_weight         1010.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                114.818(2)
_cell_angle_beta                 91.946(2)
_cell_angle_gamma                96.673(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9668(5)
_cell_length_b                   11.9630(5)
_cell_length_c                   12.1132(6)
_cell_measurement_reflns_used    3914
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      31.2781
_cell_measurement_theta_min      2.4688
_cell_volume                     1426.61(12)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'APEX3 (Bruker AXS Inc., 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2018)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Photon II CPADs detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Multilayer Mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_av_unetI/netI     0.0972
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24979
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.47
_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Bruker D8 Quest'
_exptl_absorpt_coefficient_mu    15.861
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.28
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.587
_refine_diff_density_min         -1.358
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         7552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0462
_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)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0727
_reflns_number_gt                5173
_reflns_number_total             7552
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm9b03925_si_002.cif
_cod_data_source_block           5[PbBr3]
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C20 H32 Br5 N2 Pb1.50'
_cod_database_code               4003556
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br Br1 1.09610(7) 0.08888(7) 0.68562(7) 0.02317(18) Uani d . . . 1 . .
Br Br2 0.74663(7) 0.12794(8) 0.63324(7) 0.02409(18) Uani d . . . 1 . .
Br Br3 0.78766(7) 0.29370(7) 0.41177(7) 0.02211(17) Uani d . . . 1 . .
Br Br4 0.84541(7) 0.70580(8) 0.61398(7) 0.0296(2) Uani d . . . 1 . .
Br Br5 0.97425(7) 0.55840(7) 0.28045(7) 0.02439(18) Uani d . . . 1 . .
C C1 0.5490(7) 0.3555(8) 0.6121(7) 0.0244(18) Uani d . . . 1 . .
H H1 0.612379 0.30463 0.587216 0.029 Uiso calc U . R 1 . .
C C2 0.5719(7) 0.4765(8) 0.6317(7) 0.030(2) Uani d . . . 1 . .
H H2 0.651047 0.510929 0.621897 0.036 Uiso calc U . R 1 . .
C C3 0.4789(8) 0.5486(8) 0.6659(7) 0.033(2) Uani d . . . 1 . .
H H3 0.49322 0.633147 0.6785 0.04 Uiso calc U . R 1 . .
C C4 0.3653(8) 0.4988(8) 0.6821(7) 0.030(2) Uani d . . . 1 . .
H H4 0.300885 0.548402 0.706676 0.036 Uiso calc U . R 1 . .
C C5 0.3464(7) 0.3754(8) 0.6618(7) 0.0271(19) Uani d . . . 1 . .
H H5 0.268283 0.339471 0.672398 0.033 Uiso calc U . R 1 . .
C C6 0.4166(7) 0.1750(7) 0.6119(7) 0.0267(19) Uani d . . . 1 . .
H H6A 0.473182 0.126642 0.554356 0.032 Uiso calc U . R 1 . .
H H6B 0.330949 0.13715 0.576964 0.032 Uiso calc U . R 1 . .
C C7 0.4390(7) 0.1699(7) 0.7325(7) 0.0204(17) Uani d . . . 1 . .
H H7A 0.37298 0.205261 0.784702 0.024 Uiso calc U . R 1 . .
H H7B 0.518519 0.221494 0.774242 0.024 Uiso calc U . R 1 . .
C C8 0.4419(7) 0.0368(7) 0.7172(7) 0.0251(18) Uani d . . . 1 . .
H H8A 0.359385 -0.012353 0.683679 0.03 Uiso calc U . R 1 . .
H H8B 0.501361 -0.001588 0.657707 0.03 Uiso calc U . R 1 . .
C C9 0.4781(7) 0.0311(8) 0.8369(7) 0.030(2) Uani d . . . 1 . .
H H9A 0.415194 0.063746 0.894382 0.036 Uiso calc U . R 1 . .
H H9B 0.557696 0.085234 0.873521 0.036 Uiso calc U . R 1 . .
C C10 0.4902(8) -0.1020(7) 0.8202(8) 0.034(2) Uani d . . . 1 . .
H H10A 0.410662 -0.155347 0.787219 0.051 Uiso calc U . R 1 . .
H H10B 0.515296 -0.100513 0.899266 0.051 Uiso calc U . R 1 . .
H H10C 0.552401 -0.134931 0.763349 0.051 Uiso calc U . R 1 . .
C C11 0.8451(7) 0.0662(8) 0.8942(7) 0.0283(19) Uani d . . . 1 . .
H H11 0.831626 0.058577 0.813271 0.034 Uiso calc U . R 1 . .
C C12 0.8250(7) -0.0379(7) 0.9160(7) 0.0256(18) Uani d . . . 1 . .
H H12 0.799153 -0.117525 0.850712 0.031 Uiso calc U . R 1 . .
C C13 0.8428(7) -0.0252(8) 1.0340(8) 0.031(2) Uani d . . . 1 . .
H H13 0.826858 -0.095868 1.050995 0.037 Uiso calc U . R 1 . .
C C14 0.8840(7) 0.0907(8) 1.1276(7) 0.0258(18) Uani d . . . 1 . .
H H14 0.899678 0.100154 1.20893 0.031 Uiso calc U . R 1 . .
C C15 0.9018(7) 0.1913(8) 1.1011(7) 0.0275(19) Uani d . . . 1 . .
H H15 0.927473 0.271664 1.165248 0.033 Uiso calc U . R 1 . .
C C16 0.8984(7) 0.2926(7) 0.9629(7) 0.0238(18) Uani d . . . 1 . .
H H16A 0.923521 0.271357 0.879531 0.029 Uiso calc U . R 1 . .
H H16B 0.963456 0.355871 1.021974 0.029 Uiso calc U . R 1 . .
C C17 0.7776(7) 0.3447(7) 0.9757(7) 0.0245(18) Uani d . . . 1 . .
H H17A 0.750086 0.360822 1.057367 0.029 Uiso calc U . R 1 . .
H H17B 0.713835 0.282833 0.913488 0.029 Uiso calc U . R 1 . .
C C18 0.7916(7) 0.4648(7) 0.9598(7) 0.0275(19) Uani d . . . 1 . .
H H18A 0.852201 0.527494 1.025083 0.033 Uiso calc U . R 1 . .
H H18B 0.825056 0.449151 0.880487 0.033 Uiso calc U . R 1 . .
C C19 0.6717(7) 0.5178(8) 0.9637(7) 0.030(2) Uani d . . . 1 . .
H H19A 0.634338 0.527563 1.039881 0.036 Uiso calc U . R 1 . .
H H19B 0.613276 0.459 0.893815 0.036 Uiso calc U . R 1 . .
C C20 0.6935(9) 0.6441(8) 0.9582(8) 0.039(2) Uani d . . . 1 . .
H H20A 0.753094 0.70162 1.025963 0.058 Uiso calc U . R 1 . .
H H20B 0.615418 0.677847 0.964493 0.058 Uiso calc U . R 1 . .
H H20C 0.725779 0.633583 0.880483 0.058 Uiso calc U . R 1 . .
N N1 0.4370(6) 0.3065(6) 0.6275(5) 0.0212(14) Uani d . . . 1 . .
N N2 0.8839(6) 0.1788(6) 0.9862(6) 0.0229(15) Uani d . . . 1 . .
Pb Pb1 0.95381(3) 0.17674(3) 0.52492(3) 0.01946(8) Uani d . . . 1 . .
Pb Pb2 1.0 0.5 0.5 0.02135(10) Uani d . P S 1 . .
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'
Pb Pb -3.3944 10.1111 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Pb1 Br1 Pb1 . 2_756 88.01(2) ?
Pb2 Br3 Pb1 . . 82.746(19) ?
Pb2 Br5 Pb1 . 2_766 81.89(2) ?
N1 C1 C2 . . 120.7(8) ?
N1 C1 H1 . . 119.7 ?
C2 C1 H1 . . 119.7 ?
C1 C2 C3 . . 119.1(8) ?
C1 C2 H2 . . 120.5 ?
C3 C2 H2 . . 120.5 ?
C4 C3 C2 . . 120.2(8) ?
C4 C3 H3 . . 119.9 ?
C2 C3 H3 . . 119.9 ?
C3 C4 C5 . . 118.8(8) ?
C3 C4 H4 . . 120.6 ?
C5 C4 H4 . . 120.6 ?
N1 C5 C4 . . 120.3(8) ?
N1 C5 H5 . . 119.9 ?
C4 C5 H5 . . 119.9 ?
N1 C6 C7 . . 110.4(6) ?
N1 C6 H6A . . 109.6 ?
C7 C6 H6A . . 109.6 ?
N1 C6 H6B . . 109.6 ?
C7 C6 H6B . . 109.6 ?
H6A C6 H6B . . 108.1 ?
C6 C7 C8 . . 111.8(6) ?
C6 C7 H7A . . 109.3 ?
C8 C7 H7A . . 109.3 ?
C6 C7 H7B . . 109.3 ?
C8 C7 H7B . . 109.3 ?
H7A C7 H7B . . 107.9 ?
C9 C8 C7 . . 112.5(7) ?
C9 C8 H8A . . 109.1 ?
C7 C8 H8A . . 109.1 ?
C9 C8 H8B . . 109.1 ?
C7 C8 H8B . . 109.1 ?
H8A C8 H8B . . 107.8 ?
C8 C9 C10 . . 112.6(7) ?
C8 C9 H9A . . 109.1 ?
C10 C9 H9A . . 109.1 ?
C8 C9 H9B . . 109.1 ?
C10 C9 H9B . . 109.1 ?
H9A C9 H9B . . 107.8 ?
C9 C10 H10A . . 109.5 ?
C9 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C9 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
N2 C11 C12 . . 120.7(7) ?
N2 C11 H11 . . 119.7 ?
C12 C11 H11 . . 119.7 ?
C11 C12 C13 . . 119.0(8) ?
C11 C12 H12 . . 120.5 ?
C13 C12 H12 . . 120.5 ?
C12 C13 C14 . . 119.9(8) ?
C12 C13 H13 . . 120.1 ?
C14 C13 H13 . . 120.1 ?
C15 C14 C13 . . 118.8(8) ?
C15 C14 H14 . . 120.6 ?
C13 C14 H14 . . 120.6 ?
N2 C15 C14 . . 121.3(8) ?
N2 C15 H15 . . 119.4 ?
C14 C15 H15 . . 119.4 ?
N2 C16 C17 . . 109.7(6) ?
N2 C16 H16A . . 109.7 ?
C17 C16 H16A . . 109.7 ?
N2 C16 H16B . . 109.7 ?
C17 C16 H16B . . 109.7 ?
H16A C16 H16B . . 108.2 ?
C16 C17 C18 . . 110.9(6) ?
C16 C17 H17A . . 109.5 ?
C18 C17 H17A . . 109.5 ?
C16 C17 H17B . . 109.5 ?
C18 C17 H17B . . 109.5 ?
H17A C17 H17B . . 108.1 ?
C19 C18 C17 . . 113.5(7) ?
C19 C18 H18A . . 108.9 ?
C17 C18 H18A . . 108.9 ?
C19 C18 H18B . . 108.9 ?
C17 C18 H18B . . 108.9 ?
H18A C18 H18B . . 107.7 ?
C18 C19 C20 . . 111.1(7) ?
C18 C19 H19A . . 109.4 ?
C20 C19 H19A . . 109.4 ?
C18 C19 H19B . . 109.4 ?
C20 C19 H19B . . 109.4 ?
H19A C19 H19B . . 108.0 ?
C19 C20 H20A . . 109.5 ?
C19 C20 H20B . . 109.5 ?
H20A C20 H20B . . 109.5 ?
C19 C20 H20C . . 109.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 109.5 ?
C5 N1 C1 . . 121.0(7) ?
C5 N1 C6 . . 119.5(7) ?
C1 N1 C6 . . 119.5(7) ?
C15 N2 C11 . . 120.4(7) ?
C15 N2 C16 . . 119.1(7) ?
C11 N2 C16 . . 120.4(6) ?
Br2 Pb1 Br3 . . 85.66(2) ?
Br2 Pb1 Br1 . . 86.02(2) ?
Br3 Pb1 Br1 . . 168.27(2) ?
Br2 Pb1 Br5 . 2_766 94.60(2) ?
Br3 Pb1 Br5 . 2_766 84.22(2) ?
Br1 Pb1 Br5 . 2_766 88.22(2) ?
Br2 Pb1 Br1 . 2_756 91.14(2) ?
Br3 Pb1 Br1 . 2_756 96.42(2) ?
Br1 Pb1 Br1 . 2_756 91.99(2) ?
Br5 Pb1 Br1 2_766 2_756 174.26(2) ?
Br3 Pb2 Br3 . 2_766 180.0 ?
Br3 Pb2 Br4 . 2_766 84.65(2) ?
Br3 Pb2 Br4 2_766 2_766 95.35(2) ?
Br3 Pb2 Br4 . . 95.35(2) ?
Br3 Pb2 Br4 2_766 . 84.65(2) ?
Br4 Pb2 Br4 2_766 . 180.0 ?
Br3 Pb2 Br5 . 2_766 85.08(2) ?
Br3 Pb2 Br5 2_766 2_766 94.92(2) ?
Br4 Pb2 Br5 2_766 2_766 84.05(2) ?
Br4 Pb2 Br5 . 2_766 95.95(2) ?
Br3 Pb2 Br5 . . 94.92(2) ?
Br3 Pb2 Br5 2_766 . 85.08(2) ?
Br4 Pb2 Br5 2_766 . 95.95(2) ?
Br4 Pb2 Br5 . . 84.05(2) ?
Br5 Pb2 Br5 2_766 . 180.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Br1 Pb1 . 3.0367(8) ?
Br1 Pb1 2_756 3.0982(9) ?
Br2 Pb1 . 2.7861(8) ?
Br3 Pb2 . 2.9895(8) ?
Br3 Pb1 . 3.0314(8) ?
Br4 Pb2 . 3.0195(8) ?
Br5 Pb2 . 3.0323(8) ?
Br5 Pb1 2_766 3.0401(9) ?
C1 N1 . 1.353(9) ?
C1 C2 . 1.355(11) ?
C1 H1 . 0.95 ?
C2 C3 . 1.375(11) ?
C2 H2 . 0.95 ?
C3 C4 . 1.374(11) ?
C3 H3 . 0.95 ?
C4 C5 . 1.380(11) ?
C4 H4 . 0.95 ?
C5 N1 . 1.331(9) ?
C5 H5 . 0.95 ?
C6 N1 . 1.492(9) ?
C6 C7 . 1.501(9) ?
C6 H6A . 0.99 ?
C6 H6B . 0.99 ?
C7 C8 . 1.528(10) ?
C7 H7A . 0.99 ?
C7 H7B . 0.99 ?
C8 C9 . 1.521(10) ?
C8 H8A . 0.99 ?
C8 H8B . 0.99 ?
C9 C10 . 1.541(10) ?
C9 H9A . 0.99 ?
C9 H9B . 0.99 ?
C10 H10A . 0.98 ?
C10 H10B . 0.98 ?
C10 H10C . 0.98 ?
C11 N2 . 1.347(10) ?
C11 C12 . 1.374(11) ?
C11 H11 . 0.95 ?
C12 C13 . 1.376(10) ?
C12 H12 . 0.95 ?
C13 C14 . 1.383(11) ?
C13 H13 . 0.95 ?
C14 C15 . 1.365(11) ?
C14 H14 . 0.95 ?
C15 N2 . 1.342(9) ?
C15 H15 . 0.95 ?
C16 N2 . 1.493(9) ?
C16 C17 . 1.514(10) ?
C16 H16A . 0.99 ?
C16 H16B . 0.99 ?
C17 C18 . 1.520(10) ?
C17 H17A . 0.99 ?
C17 H17B . 0.99 ?
C18 C19 . 1.518(10) ?
C18 H18A . 0.99 ?
C18 H18B . 0.99 ?
C19 C20 . 1.532(11) ?
C19 H19A . 0.99 ?
C19 H19B . 0.99 ?
C20 H20A . 0.98 ?
C20 H20B . 0.98 ?
C20 H20C . 0.98 ?
