#------------------------------------------------------------------------------
#$Date: 2020-05-22 01:21:03 +0300 (Fri, 22 May 2020) $
#$Revision: 252250 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/35/4003554.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_4003554
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            'C12 H12 I3 N Pb'
_chemical_formula_weight         758.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 101.304(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7951(11)
_cell_length_b                   7.8822(7)
_cell_length_c                   11.8001(11)
_cell_measurement_reflns_used    2975
_cell_measurement_temperature    296.(2)
_cell_measurement_theta_max      27.3982
_cell_measurement_theta_min      2.7231
_cell_volume                     1075.79(17)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0950
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20470
_diffrn_reflns_theta_full        32.65
_diffrn_reflns_theta_max         32.65
_diffrn_reflns_theta_min         2.72
_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Bruker D8 Quest'
_exptl_absorpt_coefficient_mu    12.132
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.39
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.619
_refine_diff_density_min         -1.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         4177
_refine_ls_number_restraints     261
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1407
_refine_ls_R_factor_gt           0.0554
_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)+(0.0816P)²+0.1230P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1769
_reflns_number_gt                1976
_reflns_number_total             4177
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm9b03925_si_002.cif
_cod_data_source_block           1[PbI3]
_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               4003554
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
C C1 0.9306(15) 0.121(2) 0.3058(16) 0.106(5) Uani d U P DG 0.5 A -1
H H1 0.900481 0.015886 0.279454 0.127 Uiso calc U P R 0.5 A -1
C C2 1.0494(14) 0.142(2) 0.3400(18) 0.112(5) Uani d U P G 0.5 A -1
H H2 1.098781 0.050623 0.336642 0.134 Uiso calc U P R 0.5 A -1
C C3 1.0945(11) 0.299(3) 0.3793(17) 0.114(5) Uani d U P G 0.5 A -1
H H3 1.174017 0.312615 0.402271 0.137 Uiso calc U P R 0.5 A -1
C C4 1.0208(16) 0.435(2) 0.3844(18) 0.113(5) Uani d U P G 0.5 A -1
H H4 1.050952 0.539872 0.410714 0.135 Uiso calc U P R 0.5 A -1
C C5 0.9020(15) 0.414(3) 0.3501(17) 0.106(5) Uani d U P DG 0.5 A -1
H H5 0.852652 0.505139 0.353527 0.127 Uiso calc U P R 0.5 A -1
C C6 0.8569(10) 0.257(3) 0.3108(14) 0.097(4) Uani d U P G 0.5 A -1
C C7 0.7285(14) 0.241(5) 0.2689(14) 0.101(4) Uani d U P D 0.5 A -1
H H7A 0.702395 0.139712 0.302816 0.121 Uiso calc U P R 0.5 A -1
H H7B 0.691354 0.337362 0.297621 0.121 Uiso calc U P R 0.5 A -1
N N1 0.6881(13) 0.232(3) 0.1407(11) 0.109(4) Uani d U P G 0.5 A -1
C C8 0.6502(19) 0.077(3) 0.0916(15) 0.117(5) Uani d U P DG 0.5 A -1
H H8 0.648311 -0.017651 0.138476 0.14 Uiso calc U P R 0.5 A -1
C C9 0.615(2) 0.063(3) -0.0275(16) 0.122(6) Uani d U P G 0.5 A -1
H H9 0.589609 -0.041215 -0.060365 0.146 Uiso calc U P R 0.5 A -1
C C10 0.6177(17) 0.204(3) -0.0975(11) 0.125(6) Uani d U P G 0.5 A -1
H H10 0.594199 0.194371 -0.177237 0.149 Uiso calc U P R 0.5 A -1
C C11 0.656(2) 0.359(2) -0.0484(15) 0.121(6) Uani d U P G 0.5 A -1
H H11 0.657493 0.453523 -0.095269 0.145 Uiso calc U P R 0.5 A -1
C C12 0.6908(18) 0.373(2) 0.0707(16) 0.114(5) Uani d U P DG 0.5 A -1
H H12 0.716196 0.47709 0.103572 0.137 Uiso calc U P R 0.5 A -1
I I1 0.41616(10) 0.25 0.28567(9) 0.0662(3) Uani d T P S 1 . .
I I2 0.28563(9) 0.75 0.41591(10) 0.0662(3) Uani d T P S 1 . .
I I3 0.35959(10) 0.25 0.64047(10) 0.0659(3) Uani d T P S 1 . .
Pb Pb1 0.5 0.5 0.5 0.0512(2) 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'
I I -0.4742 1.8119 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 C6 . . 120.0 ?
C2 C1 H1 . . 120.0 ?
C6 C1 H1 . . 120.0 ?
C3 C2 C1 . . 120.0 ?
C3 C2 H2 . . 120.0 ?
C1 C2 H2 . . 120.0 ?
C2 C3 C4 . . 120.0 ?
C2 C3 H3 . . 120.0 ?
C4 C3 H3 . . 120.0 ?
C5 C4 C3 . . 120.0 ?
C5 C4 H4 . . 120.0 ?
C3 C4 H4 . . 120.0 ?
C4 C5 C6 . . 120.0 ?
C4 C5 H5 . . 120.0 ?
C6 C5 H5 . . 120.0 ?
C5 C6 C1 . . 120.0 ?
C5 C6 C7 . . 118.6(8) ?
C1 C6 C7 . . 121.3(8) ?
N1 C7 C6 . . 115.9(15) ?
N1 C7 H7A . . 108.3 ?
C6 C7 H7A . . 108.3 ?
N1 C7 H7B . . 108.3 ?
C6 C7 H7B . . 108.3 ?
H7A C7 H7B . . 107.4 ?
C8 N1 C12 . . 120.0 ?
C8 N1 C7 . . 118.4(8) ?
C12 N1 C7 . . 121.5(8) ?
N1 C8 C9 . . 120.0 ?
N1 C8 H8 . . 120.0 ?
C9 C8 H8 . . 120.0 ?
C8 C9 C10 . . 120.0 ?
C8 C9 H9 . . 120.0 ?
C10 C9 H9 . . 120.0 ?
C11 C10 C9 . . 120.0 ?
C11 C10 H10 . . 120.0 ?
C9 C10 H10 . . 120.0 ?
C10 C11 C12 . . 120.0 ?
C10 C11 H11 . . 120.0 ?
C12 C11 H11 . . 120.0 ?
C11 C12 N1 . . 120.0 ?
C11 C12 H12 . . 120.0 ?
N1 C12 H12 . . 120.0 ?
Pb1 I1 Pb1 . 2_646 75.86(2) ?
Pb1 I2 Pb1 2_656 . 75.86(2) ?
Pb1 I3 Pb1 2_646 . 75.12(2) ?
I1 Pb1 I1 . 3_666 180.0 ?
I1 Pb1 I2 . . 91.78(2) ?
I1 Pb1 I2 3_666 . 88.22(2) ?
I1 Pb1 I2 . 3_666 88.22(2) ?
I1 Pb1 I2 3_666 3_666 91.78(2) ?
I2 Pb1 I2 . 3_666 180.0 ?
I1 Pb1 I3 . 3_666 94.59(3) ?
I1 Pb1 I3 3_666 3_666 85.41(3) ?
I2 Pb1 I3 . 3_666 85.35(3) ?
I2 Pb1 I3 3_666 3_666 94.65(2) ?
I1 Pb1 I3 . . 85.41(3) ?
I1 Pb1 I3 3_666 . 94.59(3) ?
I2 Pb1 I3 . . 94.65(3) ?
I2 Pb1 I3 3_666 . 85.35(2) ?
I3 Pb1 I3 3_666 . 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
C1 C2 . 1.39 ?
C1 C6 . 1.39 ?
C1 H1 . 0.93 ?
C2 C3 . 1.39 ?
C2 H2 . 0.93 ?
C3 C4 . 1.39 ?
C3 H3 . 0.93 ?
C4 C5 . 1.39 ?
C4 H4 . 0.93 ?
C5 C6 . 1.39 ?
C5 H5 . 0.93 ?
C6 C7 . 1.504(15) ?
C7 N1 . 1.496(15) ?
C7 H7A . 0.97 ?
C7 H7B . 0.97 ?
N1 C8 . 1.39 ?
N1 C12 . 1.39 ?
C8 C9 . 1.39 ?
C8 H8 . 0.93 ?
C9 C10 . 1.39 ?
C9 H9 . 0.93 ?
C10 C11 . 1.39 ?
C10 H10 . 0.93 ?
C11 C12 . 1.39 ?
C11 H11 . 0.93 ?
C12 H12 . 0.93 ?
I1 Pb1 . 3.2058(8) ?
I1 Pb1 2_646 3.2058(8) ?
I2 Pb1 2_656 3.2059(9) ?
I2 Pb1 . 3.2059(9) ?
I3 Pb1 2_646 3.2326(8) ?
I3 Pb1 . 3.2326(8) ?
