#------------------------------------------------------------------------------
#$Date: 2017-10-31 04:40:24 +0200 (Tue, 31 Oct 2017) $
#$Revision: 202433 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/08/7120837.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_7120837
loop_
_publ_author_name
'Liu, Guangfeng'
'Gu, Peiyang'
'NIE, Lina'
'zhang, qichun'
_publ_section_title
;
 Simultaneous Crystallization of in situ Formed Conjugated Polymer and
 Inorganic Matrix for Structure Solving
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06620A
_journal_year                    2017
_chemical_formula_sum            'C5 H6 Br3 N O Pb'
_chemical_formula_weight         543.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-08-01 deposited with the CCDC.
2017-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                103.012(2)
_cell_angle_beta                 97.348(2)
_cell_angle_gamma                94.651(2)
_cell_formula_units_Z            2
_cell_length_a                   4.3093(8)
_cell_length_b                   10.586(2)
_cell_length_c                   12.335(2)
_cell_measurement_reflns_used    5888
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.29
_cell_volume                     540.22(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2481
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.547
_diffrn_reflns_theta_min         1.987
_exptl_absorpt_coefficient_mu    26.660
_exptl_absorpt_correction_T_max  0.094913
_exptl_absorpt_correction_T_min  0.016785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker TWINABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.338
_exptl_crystal_description       prism
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.101
_refine_diff_density_max         1.191
_refine_diff_density_min         -2.118
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2481
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0368
_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)+(0.0605P)²+0.3663P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2112
_reflns_number_total             2481
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cc06620a3.cif
_cod_data_source_block           liujie201719_0m_5
_cod_original_cell_volume        540.23(18)
_cod_database_code               7120837
_shelx_shelxl_version_number     2014/7
_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_min   0.071
_shelx_estimated_absorpt_t_max   0.174
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Pb1 Pb 0.28773(7) 0.68451(3) 0.60486(2) 0.03945(13) Uani 1 1 d . .
N1 N 0.910(3) 0.8508(8) 0.2676(7) 0.0704(5) Uani 1 1 d . U
H6 H 0.9096 0.8978 0.3342 0.084 Uiso 1 1 calc R U
Br1 Br 0.7658(2) 0.50092(8) 0.65295(7) 0.0462(2) Uani 1 1 d . .
O1 O 0.901(2) 0.6337(7) -0.0471(5) 0.0705(5) Uani 1 1 d . U
H3 H 1.0376 0.6649 -0.0770 0.106 Uiso 1 1 calc R U
C1 C 0.775(3) 0.7248(10) 0.2394(8) 0.0704(5) Uani 1 1 d . U
H1 H 0.6873 0.6890 0.2925 0.084 Uiso 1 1 calc R U
C2 C 0.767(3) 0.6517(11) 0.1329(8) 0.0704(5) Uani 1 1 d . U
H2 H 0.6739 0.5658 0.1119 0.085 Uiso 1 1 calc R U
Br2 Br 0.3979(2) 0.82372(10) 0.83017(8) 0.0585(3) Uani 1 1 d . .
C3 C 0.903(3) 0.7083(10) 0.0562(8) 0.0704(5) Uani 1 1 d . U
Br3 Br -0.2123(2) 0.85437(8) 0.54003(7) 0.0460(2) Uani 1 1 d . .
C4 C 1.033(3) 0.8351(10) 0.0861(8) 0.0704(5) Uani 1 1 d . U
H4 H 1.1121 0.8751 0.0340 0.085 Uiso 1 1 calc R U
C5 C 1.042(3) 0.9012(11) 0.1950(8) 0.0704(5) Uani 1 1 d . U
H5 H 1.1453 0.9854 0.2185 0.084 Uiso 1 1 calc R U
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Br2 Pb1 Br3 93.10(3) . 1_655
Br2 Pb1 Br1 91.06(3) . .
Br3 Pb1 Br1 90.21(3) 1_655 .
Br2 Pb1 Br1 91.06(3) . 1_455
Br3 Pb1 Br1 175.84(2) 1_655 1_455
Br1 Pb1 Br1 90.00(3) . 1_455
Br2 Pb1 Br3 93.04(3) . .
Br3 Pb1 Br3 90.76(3) 1_655 .
Br1 Pb1 Br3 175.73(2) . .
Br1 Pb1 Br3 88.72(3) 1_455 .
C5 N1 C1 120.9(9) . .
C5 N1 H6 119.5 . .
C1 N1 H6 119.5 . .
Pb1 Br1 Pb1 90.01(3) . 1_655
C3 O1 H3 109.5 . .
C2 C1 N1 119.5(10) . .
C2 C1 H1 120.3 . .
N1 C1 H1 120.3 . .
C1 C2 C3 118.6(11) . .
C1 C2 H2 120.7 . .
C3 C2 H2 120.7 . .
O1 C3 C4 121.7(10) . .
O1 C3 C2 117.6(10) . .
C4 C3 C2 120.7(10) . .
Pb1 Br3 Pb1 90.76(3) 1_455 .
C3 C4 C5 117.6(10) . .
C3 C4 H4 121.2 . .
C5 C4 H4 121.2 . .
N1 C5 C4 122.5(11) . .
N1 C5 H5 118.7 . .
C4 C5 H5 118.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 Br2 2.7974(11) .
Pb1 Br3 2.9959(9) 1_655
Pb1 Br1 3.0380(10) .
Pb1 Br1 3.0560(9) 1_455
Pb1 Br3 3.0578(10) .
N1 C5 1.305(14) .
N1 C1 1.362(13) .
N1 H6 0.8600 .
Br1 Pb1 3.0560(9) 1_655
O1 C3 1.338(11) .
O1 H3 0.8200 .
C1 C2 1.361(13) .
C1 H1 0.9300 .
C2 C3 1.391(15) .
C2 H2 0.9300 .
C3 C4 1.361(15) .
Br3 Pb1 2.9959(9) 1_455
C4 C5 1.362(13) .
C4 H4 0.9300 .
C5 H5 0.9300 .
