#------------------------------------------------------------------------------
#$Date: 2020-05-22 01:21:03 +0300 (Fri, 22 May 2020) $
#$Revision: 252250 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/35/4003557.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_4003557
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            'C7 H7 Br3 N O Pb'
_chemical_formula_weight         568.06
_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                90.295(2)
_cell_angle_beta                 98.934(2)
_cell_angle_gamma                100.308(2)
_cell_formula_units_Z            4
_cell_length_a                   7.7918(7)
_cell_length_b                   11.1156(9)
_cell_length_c                   14.7794(12)
_cell_measurement_reflns_used    4364
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      33.2024
_cell_measurement_theta_min      2.7895
_cell_volume                     1243.40(18)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0957
_diffrn_reflns_av_unetI/netI     0.1038
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10746
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         2.29
_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Bruker D8 Quest'
_exptl_absorpt_coefficient_mu    23.174
_exptl_absorpt_correction_T_max  0.65
_exptl_absorpt_correction_T_min  0.17
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.035
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.234
_refine_diff_density_min         -3.517
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         10746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0368P)²+3.1667P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                6773
_reflns_number_total             10746
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm9b03925_si_002.cif
_cod_data_source_block           6[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_database_code               4003557
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 0.63733(13) 0.11648(8) 0.33185(6) 0.02022(18) Uani d . . . 1 . .
Br Br2 0.62248(13) 0.30182(9) 0.08863(6) 0.02338(19) Uani d . . . 1 . .
Br Br3 0.14232(13) 0.10679(8) 0.15035(6) 0.02046(18) Uani d . . . 1 . .
Br Br4 0.20191(12) 0.26748(9) 0.40130(6) 0.02014(18) Uani d . . . 1 . .
Br Br5 0.18076(13) 0.46406(8) 0.16726(6) 0.02173(19) Uani d . . . 1 . .
Br Br6 -0.21609(13) 0.47700(9) 0.32176(6) 0.02166(19) Uani d . . . 1 . .
C C1 0.5938(13) 0.6994(9) 0.1411(6) 0.0203(18) Uani d . . . 1 . .
H H1 0.590544 0.615128 0.152988 0.024 Uiso calc U . R 1 . .
C C2 0.4736(13) 0.7598(10) 0.1720(7) 0.028(2) Uani d . . . 1 . .
H H2 0.384168 0.716773 0.202852 0.033 Uiso calc U . R 1 . .
C C3 0.4838(13) 0.8823(10) 0.1581(7) 0.027(2) Uani d . . . 1 . .
H H3 0.406042 0.925981 0.182394 0.033 Uiso calc U . R 1 . .
C C4 0.6058(13) 0.9414(9) 0.1091(6) 0.0233(19) Uani d . . . 1 . .
H H4 0.608794 1.025127 0.095476 0.028 Uiso calc U . R 1 . .
C C5 0.7249(13) 0.8782(9) 0.0796(6) 0.0224(19) Uani d . . . 1 . .
H H5 0.814647 0.919999 0.048392 0.027 Uiso calc U . R 1 . .
C C6 0.8421(12) 0.6935(8) 0.0576(6) 0.0197(18) Uani d . . . 1 . .
H H6A 0.835969 0.70671 -0.008923 0.024 Uiso calc U . R 1 . .
H H6B 0.80922 0.604551 0.066281 0.024 Uiso calc U . R 1 . .
C C7 1.0273(13) 0.7389(9) 0.1055(6) 0.0223(19) Uani d . . . 1 . .
H H7A 1.109426 0.697344 0.077526 0.027 Uiso calc U . R 1 . .
H H7B 1.059384 0.827709 0.096146 0.027 Uiso calc U . R 1 . .
C C8 0.1536(12) 0.6947(8) 0.4482(6) 0.0178(17) Uani d . . . 1 . .
H H8 0.039625 0.673957 0.465236 0.021 Uiso calc U . R 1 . .
C C9 0.2505(15) 0.6072(10) 0.4371(7) 0.027(2) Uani d . . . 1 . .
H H9 0.201652 0.523788 0.444278 0.032 Uiso calc U . R 1 . .
C C10 0.4165(15) 0.6368(11) 0.4158(6) 0.032(3) Uani d . . . 1 . .
H H10 0.485318 0.575416 0.410631 0.038 Uiso calc U . R 1 . .
C C11 0.4834(14) 0.7586(12) 0.4018(6) 0.033(3) Uani d . . . 1 . .
H H11 0.598533 0.781275 0.386489 0.04 Uiso calc U . R 1 . .
C C12 0.3845(15) 0.8440(10) 0.4101(7) 0.030(2) Uani d . . . 1 . .
H H12 0.428295 0.927005 0.398696 0.035 Uiso calc U . R 1 . .
C C13 0.1144(14) 0.9082(8) 0.4427(6) 0.024(2) Uani d . . . 1 . .
H H13A 0.192533 0.987123 0.462986 0.028 Uiso calc U . R 1 . .
H H13B 0.037334 0.884756 0.48946 0.028 Uiso calc U . R 1 . .
C C14 0.0011(14) 0.9227(9) 0.3511(6) 0.024(2) Uani d . . . 1 . .
H H14A -0.058654 0.993469 0.35555 0.029 Uiso calc U . R 1 . .
H H14B 0.07748 0.939059 0.303253 0.029 Uiso calc U . R 1 . .
N N1 0.7155(11) 0.7587(7) 0.0944(5) 0.0211(16) Uani d . . . 1 . .
N N2 0.2238(9) 0.8126(7) 0.4344(5) 0.0167(14) Uani d . . . 1 . .
O O1 1.0487(10) 0.7182(6) 0.2011(4) 0.0232(14) Uani d . . . 1 . .
H H1A 1.054818 0.644414 0.209867 0.035 Uiso calc U . R 1 . .
O O2 -0.1258(10) 0.8169(6) 0.3261(5) 0.0260(15) Uani d . . . 1 . .
H H2A -0.091557 0.774991 0.287352 0.039 Uiso calc U . R 1 . .
Pb Pb1 0.42895(5) 0.29016(3) 0.24723(2) 0.01731(7) Uani d . . . 1 . .
Pb Pb2 -0.07797(5) 0.28370(3) 0.24260(2) 0.01721(7) Uani d . . . 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Pb1 Br1 Pb2 . 1_655 80.18(2) ?
Pb1 Br2 Pb2 . 1_655 80.23(2) ?
Pb2 Br4 Pb1 . . 80.90(2) ?
Pb2 Br5 Pb1 . . 81.43(3) ?
Pb2 Br6 Pb1 . 1_455 78.92(3) ?
N1 C1 C2 . . 120.4(9) ?
N1 C1 H1 . . 119.8 ?
C2 C1 H1 . . 119.8 ?
C3 C2 C1 . . 119.5(9) ?
C3 C2 H2 . . 120.3 ?
C1 C2 H2 . . 120.3 ?
C4 C3 C2 . . 119.7(9) ?
C4 C3 H3 . . 120.1 ?
C2 C3 H3 . . 120.1 ?
C3 C4 C5 . . 119.2(10) ?
C3 C4 H4 . . 120.4 ?
C5 C4 H4 . . 120.4 ?
N1 C5 C4 . . 120.7(9) ?
N1 C5 H5 . . 119.6 ?
C4 C5 H5 . . 119.6 ?
N1 C6 C7 . . 110.7(7) ?
N1 C6 H6A . . 109.5 ?
C7 C6 H6A . . 109.5 ?
N1 C6 H6B . . 109.5 ?
C7 C6 H6B . . 109.5 ?
H6A C6 H6B . . 108.1 ?
O1 C7 C6 . . 112.9(8) ?
O1 C7 H7A . . 109.0 ?
C6 C7 H7A . . 109.0 ?
O1 C7 H7B . . 109.0 ?
C6 C7 H7B . . 109.0 ?
H7A C7 H7B . . 107.8 ?
N2 C8 C9 . . 118.3(9) ?
N2 C8 H8 . . 120.9 ?
C9 C8 H8 . . 120.9 ?
C8 C9 C10 . . 121.1(10) ?
C8 C9 H9 . . 119.4 ?
C10 C9 H9 . . 119.4 ?
C9 C10 C11 . . 118.8(9) ?
C9 C10 H10 . . 120.6 ?
C11 C10 H10 . . 120.6 ?
C12 C11 C10 . . 119.6(10) ?
C12 C11 H11 . . 120.2 ?
C10 C11 H11 . . 120.2 ?
C11 C12 N2 . . 120.2(10) ?
C11 C12 H12 . . 119.9 ?
N2 C12 H12 . . 119.9 ?
N2 C13 C14 . . 110.5(7) ?
N2 C13 H13A . . 109.6 ?
C14 C13 H13A . . 109.6 ?
N2 C13 H13B . . 109.6 ?
C14 C13 H13B . . 109.6 ?
H13A C13 H13B . . 108.1 ?
O2 C14 C13 . . 110.8(8) ?
O2 C14 H14A . . 109.5 ?
C13 C14 H14A . . 109.5 ?
O2 C14 H14B . . 109.5 ?
C13 C14 H14B . . 109.5 ?
H14A C14 H14B . . 108.1 ?
C5 N1 C1 . . 120.4(8) ?
C5 N1 C6 . . 118.6(8) ?
C1 N1 C6 . . 120.9(8) ?
C12 N2 C8 . . 121.9(8) ?
C12 N2 C13 . . 119.8(9) ?
C8 N2 C13 . . 118.3(8) ?
C7 O1 H1A . . 109.5 ?
C14 O2 H2A . . 109.5 ?
Br1 Pb1 Br3 . . 95.86(3) ?
Br1 Pb1 Br2 . . 89.84(3) ?
Br3 Pb1 Br2 . . 91.16(3) ?
Br1 Pb1 Br4 . . 91.81(3) ?
Br3 Pb1 Br4 . . 84.41(3) ?
Br2 Pb1 Br4 . . 175.40(3) ?
Br1 Pb1 Br5 . . 174.75(3) ?
Br3 Pb1 Br5 . . 81.71(3) ?
Br2 Pb1 Br5 . . 94.85(3) ?
Br4 Pb1 Br5 . . 83.34(3) ?
Br1 Pb1 Br6 . 1_655 81.34(3) ?
Br3 Pb1 Br6 . 1_655 168.53(3) ?
Br2 Pb1 Br6 . 1_655 77.75(3) ?
Br4 Pb1 Br6 . 1_655 106.74(3) ?
Br5 Pb1 Br6 . 1_655 101.94(3) ?
Br6 Pb2 Br5 . . 90.72(3) ?
Br6 Pb2 Br4 . . 95.97(3) ?
Br5 Pb2 Br4 . . 87.88(3) ?
Br6 Pb2 Br2 . 1_455 81.55(3) ?
Br5 Pb2 Br2 . 1_455 94.32(3) ?
Br4 Pb2 Br2 . 1_455 176.69(3) ?
Br6 Pb2 Br1 . 1_455 83.24(3) ?
Br5 Pb2 Br1 . 1_455 173.94(3) ?
Br4 Pb2 Br1 . 1_455 92.31(3) ?
Br2 Pb2 Br1 1_455 1_455 85.25(3) ?
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 . 2.9057(9) ?
Br1 Pb2 1_655 3.0942(10) ?
Br2 Pb1 . 2.9692(10) ?
Br2 Pb2 1_655 3.0315(10) ?
Br3 Pb1 . 2.9224(10) ?
Br4 Pb2 . 2.9742(10) ?
Br4 Pb1 . 3.0782(10) ?
Br5 Pb2 . 2.9321(10) ?
Br5 Pb1 . 3.0862(10) ?
Br6 Pb2 . 2.8874(9) ?
Br6 Pb1 1_455 3.1860(11) ?
C1 N1 . 1.340(12) ?
C1 C2 . 1.376(13) ?
C1 H1 . 0.95 ?
C2 C3 . 1.369(15) ?
C2 H2 . 0.95 ?
C3 C4 . 1.361(14) ?
C3 H3 . 0.95 ?
C4 C5 . 1.379(13) ?
C4 H4 . 0.95 ?
C5 N1 . 1.339(12) ?
C5 H5 . 0.95 ?
C6 N1 . 1.487(11) ?
C6 C7 . 1.502(13) ?
C6 H6A . 0.99 ?
C6 H6B . 0.99 ?
C7 O1 . 1.422(11) ?
C7 H7A . 0.99 ?
C7 H7B . 0.99 ?
C8 N2 . 1.355(11) ?
C8 C9 . 1.358(12) ?
C8 H8 . 0.95 ?
C9 C10 . 1.362(15) ?
C9 H9 . 0.95 ?
C10 C11 . 1.389(17) ?
C10 H10 . 0.95 ?
C11 C12 . 1.341(15) ?
C11 H11 . 0.95 ?
C12 N2 . 1.343(12) ?
C12 H12 . 0.95 ?
C13 N2 . 1.492(11) ?
C13 C14 . 1.524(13) ?
C13 H13A . 0.99 ?
C13 H13B . 0.99 ?
C14 O2 . 1.401(12) ?
C14 H14A . 0.99 ?
C14 H14B . 0.99 ?
O1 H1A . 0.84 ?
O2 H2A . 0.84 ?
