#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:00:24 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180407 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/76/7207629.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_7207629
loop_
_publ_author_name
'Zhang, Kou-Lin'
'Chang, Yan'
'Zhang, Jing-Bo'
'Deng, Ye'
'Qiu, Ting-Ting'
'Li, Liang'
'Ng, Seik Weng'
_publ_section_title
;
 The cosolvent-dependent assembly of a family of three blue fluorescent
 lead(ii)-coordination polymers with 5-amino-2,4,6-tribromoisophthalic
 acid
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              2926
_journal_paper_doi               10.1039/c2ce06540a
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C9 H10 Br3 N O7 Pb'
_chemical_formula_weight         691.10
_chemical_name_systematic
;
?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.7160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.0731(8)
_cell_length_b                   6.9348(6)
_cell_length_c                   11.9935(11)
_cell_measurement_reflns_used    3412
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.69
_cell_volume                     750.88(12)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'Diamond (CRYSTAL IMPACT, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6507
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    19.246
_exptl_absorpt_correction_T_max  0.260
_exptl_absorpt_correction_T_min  0.114
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.057
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.822
_refine_diff_density_min         -1.402
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0315P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0602
_reflns_number_gt                1685
_reflns_number_total             1848
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce06540a.txt
_cod_data_source_block           pb
_cod_original_sg_symbol_H-M      P21/m
_cod_database_code               7207629
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pb1 Pb 0.36382(2) 0.2500 0.52779(2) 0.02102(9) Uani 1 2 d S
Br1 Br 0.92699(8) 0.2500 0.48980(6) 0.03757(18) Uani 1 2 d S
Br2 Br 0.48324(7) 0.2500 0.12520(7) 0.03877(19) Uani 1 2 d S
Br3 Br 1.09122(7) 0.2500 0.04576(6) 0.03724(18) Uani 1 2 d S
O1 O 1.2068(3) 0.4111(4) 0.3284(3) 0.0307(7) Uani 1 1 d .
O2 O 0.5618(3) 0.0924(4) 0.4075(3) 0.0295(7) Uani 1 1 d .
O3 O 0.2413(6) 0.2500 0.7193(5) 0.0463(14) Uani 1 2 d S
H3O H 0.1384 0.2500 0.7160 0.08(4) Uiso 1 2 calc SR
O1W O 0.5926(5) 0.2500 0.6624(4) 0.0335(12) Uani 1 2 d S
H1W H 0.6366 0.1475 0.6576 0.040(16) Uiso 1 1 calc R
O2W O 0.0511(6) 0.7500 0.2381(5) 0.0426(14) Uani 1 2 d S
H2W H 0.093(7) 0.643(8) 0.270(5) 0.06(2) Uiso 1 1 d .
N1 N 0.7535(7) 0.2500 -0.0132(5) 0.0394(15) Uani 1 2 d S
H1A H 0.6614 0.2500 -0.0383 0.047 Uiso 1 2 calc SR
H1B H 0.8205 0.2500 -0.0591 0.047 Uiso 1 2 calc SR
C1 C 0.6105(6) 0.2500 0.3751(6) 0.0209(12) Uani 1 2 d S
C2 C 0.7255(6) 0.2500 0.2924(5) 0.0203(13) Uani 1 2 d S
C3 C 0.6870(6) 0.2500 0.1781(6) 0.0217(13) Uani 1 2 d S
C4 C 0.7935(7) 0.2500 0.0998(6) 0.0252(13) Uani 1 2 d S
C5 C 0.9432(6) 0.2500 0.1456(5) 0.0211(12) Uani 1 2 d S
C6 C 0.9851(6) 0.2500 0.2597(6) 0.0205(12) Uani 1 2 d S
C7 C 0.8762(7) 0.2500 0.3323(5) 0.0207(12) Uani 1 2 d S
C8 C 1.1474(7) 0.2500 0.3060(5) 0.0223(13) Uani 1 2 d S
C9 C 0.3225(10) 0.2500 0.8261(7) 0.047(2) Uani 1 2 d S
H9A H 0.2552 0.2500 0.8830 0.070 Uiso 1 2 calc SR
H9B H 0.3837 0.3630 0.8340 0.070 Uiso 0.50 1 calc PR
H9C H 0.3837 0.1370 0.8340 0.070 Uiso 0.50 1 calc PR
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'
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'
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'
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
O1W Pb1 O2 68.18(8) . 2_656
O1W Pb1 O2 68.18(8) . 3_656
O2 Pb1 O2 135.28(15) 2_656 3_656
O1W Pb1 O3 80.42(18) . .
O2 Pb1 O3 81.84(9) 2_656 .
O2 Pb1 O3 81.84(9) 3_656 .
O1W Pb1 O2 77.71(13) . .
O2 Pb1 O2 111.98(7) 2_656 .
O2 Pb1 O2 67.12(11) 3_656 .
O3 Pb1 O2 146.92(11) . .
O1W Pb1 O2 77.71(13) . 4_565
O2 Pb1 O2 67.12(11) 2_656 4_565
O2 Pb1 O2 111.98(7) 3_656 4_565
O3 Pb1 O2 146.92(11) . 4_565
O2 Pb1 O2 48.73(13) . 4_565
C1 O2 Pb1 144.0(3) . 3_656
C1 O2 Pb1 95.0(3) . .
Pb1 O2 Pb1 112.88(11) 3_656 .
C9 O3 Pb1 124.1(5) . .
C9 O3 H3O 118.0 . .
Pb1 O3 H3O 118.0 . .
Pb1 O1W H1W 109.5 . .
C4 N1 H1A 120.0 . .
C4 N1 H1B 120.0 . .
H1A N1 H1B 120.0 . .
O2 C1 O2 121.2(6) 4_565 .
O2 C1 C2 119.4(3) 4_565 .
O2 C1 C2 119.4(3) . .
C3 C2 C7 118.7(5) . .
C3 C2 C1 121.9(5) . .
C7 C2 C1 119.4(5) . .
C2 C3 C4 122.5(5) . .
C2 C3 Br2 118.3(4) . .
C4 C3 Br2 119.2(5) . .
N1 C4 C3 121.8(6) . .
N1 C4 C5 122.4(6) . .
C3 C4 C5 115.8(6) . .
C6 C5 C4 123.0(6) . .
C6 C5 Br3 119.0(4) . .
C4 C5 Br3 118.0(5) . .
C7 C6 C5 118.7(6) . .
C7 C6 C8 119.8(6) . .
C5 C6 C8 121.5(5) . .
C6 C7 C2 121.3(6) . .
C6 C7 Br1 120.6(5) . .
C2 C7 Br1 118.1(4) . .
O1 C8 O1 125.3(6) . 4_565
O1 C8 C6 117.2(3) . .
O1 C8 C6 117.2(3) 4_565 .
O3 C9 H9A 109.5 . .
O3 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
O3 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1W 2.499(5) .
Pb1 O2 2.567(3) 2_656
Pb1 O2 2.567(3) 3_656
Pb1 O3 2.649(5) .
Pb1 O2 2.650(3) .
Pb1 O2 2.650(3) 4_565
Br1 C7 1.899(6) .
Br2 C3 1.893(6) .
Br3 C5 1.887(6) .
O1 C8 1.258(4) .
O2 C1 1.255(4) .
O2 Pb1 2.567(3) 3_656
O3 C9 1.413(10) .
O3 H3O 0.9300 .
O1W H1W 0.8200 .
O2W H2W 0.91(6) .
N1 C4 1.367(9) .
N1 H1A 0.8600 .
N1 H1B 0.8600 .
C1 O2 1.255(4) 4_565
C1 C2 1.510(8) .
C2 C3 1.381(9) .
C2 C7 1.403(8) .
C3 C4 1.413(9) .
C4 C5 1.413(8) .
C5 C6 1.382(9) .
C6 C7 1.381(8) .
C6 C8 1.522(8) .
C8 O1 1.258(4) 4_565
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1W Pb1 O2 C1 -85.5(3) . .
O2 Pb1 O2 C1 -25.4(3) 2_656 .
O2 Pb1 O2 C1 -156.8(4) 3_656 .
O3 Pb1 O2 C1 -135.2(4) . .
O2 Pb1 O2 C1 -1.2(3) 4_565 .
O1W Pb1 O2 Pb1 71.28(12) . 3_656
O2 Pb1 O2 Pb1 131.41(17) 2_656 3_656
O2 Pb1 O2 Pb1 0.0 3_656 3_656
O3 Pb1 O2 Pb1 21.6(3) . 3_656
O2 Pb1 O2 Pb1 155.62(8) 4_565 3_656
O1W Pb1 O3 C9 0.000(2) . .
O2 Pb1 O3 C9 -69.11(8) 2_656 .
O2 Pb1 O3 C9 69.11(8) 3_656 .
O2 Pb1 O3 C9 49.1(2) . .
O2 Pb1 O3 C9 -49.1(2) 4_565 .
Pb1 O2 C1 O2 -139.6(3) 3_656 4_565
Pb1 O2 C1 O2 2.1(6) . 4_565
Pb1 O2 C1 C2 42.6(9) 3_656 .
Pb1 O2 C1 C2 -175.6(5) . .
O2 C1 C2 C3 -88.9(5) 4_565 .
O2 C1 C2 C3 88.9(5) . .
O2 C1 C2 C7 91.1(5) 4_565 .
O2 C1 C2 C7 -91.1(5) . .
C7 C2 C3 C4 0.0 . .
C1 C2 C3 C4 180.0 . .
C7 C2 C3 Br2 180.0 . .
C1 C2 C3 Br2 0.0 . .
C2 C3 C4 N1 180.0 . .
Br2 C3 C4 N1 0.0 . .
C2 C3 C4 C5 0.0 . .
Br2 C3 C4 C5 180.0 . .
N1 C4 C5 C6 180.0 . .
C3 C4 C5 C6 0.0 . .
N1 C4 C5 Br3 0.0 . .
C3 C4 C5 Br3 180.0 . .
C4 C5 C6 C7 0.0 . .
Br3 C5 C6 C7 180.0 . .
C4 C5 C6 C8 180.0 . .
Br3 C5 C6 C8 0.0 . .
C5 C6 C7 C2 0.0 . .
C8 C6 C7 C2 180.0 . .
C5 C6 C7 Br1 180.0 . .
C8 C6 C7 Br1 0.0 . .
C3 C2 C7 C6 0.0 . .
C1 C2 C7 C6 180.0 . .
C3 C2 C7 Br1 180.0 . .
C1 C2 C7 Br1 0.0 . .
C7 C6 C8 O1 -86.8(5) . .
C5 C6 C8 O1 93.2(5) . .
C7 C6 C8 O1 86.8(5) . 4_565
C5 C6 C8 O1 -93.2(5) . 4_565
