#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:24:14 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230485 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/76/7057627.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_7057627
loop_
_publ_author_name
'Ma, Jing-xin'
'Yang, Zhihua'
'Zhou, Tong'
'Guo, Qi'
'Yang, Jinhui'
'Yang, Tianlin'
'Yang, Qingfeng'
_publ_section_title
;
 Construction of structurally diverse luminescent lead(ii) fluorinated
 coordination polymers based on auxiliary ligands
;
_journal_issue                   18
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15413
_journal_paper_doi               10.1039/C8NJ02846J
_journal_volume                  42
_journal_year                    2018
_chemical_formula_sum            'C13 H F4 N O5 Pb'
_chemical_formula_weight         534.34
_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   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-05-22 deposited with the CCDC.
2018-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                93.629(3)
_cell_angle_beta                 103.750(9)
_cell_angle_gamma                106.323(11)
_cell_formula_units_Z            2
_cell_length_a                   7.722(2)
_cell_length_b                   8.4029(19)
_cell_length_c                   12.016(3)
_cell_measurement_reflns_used    3576
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.11
_cell_volume                     719.7(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMARTAPEX II'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8198
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.518
_diffrn_reflns_theta_min         2.551
_exptl_absorpt_coefficient_mu    11.793
_exptl_absorpt_correction_T_max  0.177
_exptl_absorpt_correction_T_min  0.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.740
_refine_diff_density_min         -1.478
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3274
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0445
_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)+(0.0381P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2830
_reflns_number_total             3274
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8nj02846j2.cif
_cod_data_source_block           p1
_cod_depositor_comments
'Adding full bibliography for 7057624--7057627.cif.'
_cod_database_code               7057627
_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   0.164
_shelx_estimated_absorpt_t_max   0.271
_shelxl_version_number           2013-2
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 0.41749(4) 1.21757(3) 0.96129(3) 0.02988(12) Uani 1 1 d . .
C1 C 0.1918(11) 0.8430(9) 1.1972(7) 0.0281(17) Uani 1 1 d . .
C2 C 0.0517(10) 0.7049(9) 1.1374(7) 0.0259(16) Uani 1 1 d . .
C3 C -0.0515(11) 0.5772(9) 1.1876(7) 0.0294(17) Uani 1 1 d . .
C4 C 0.0062(13) 0.5945(10) 1.3062(8) 0.039(2) Uani 1 1 d . .
C5 C 0.1475(14) 0.7303(11) 1.3711(8) 0.042(2) Uani 1 1 d . .
C6 C 0.2368(13) 0.8522(10) 1.3169(7) 0.037(2) Uani 1 1 d . .
C7 C 0.2829(11) 0.9811(9) 1.1355(7) 0.0277(17) Uani 1 1 d . .
C8 C -0.2241(10) 0.4423(10) 1.1171(7) 0.0302(18) Uani 1 1 d . .
C9 C 0.5770(15) 1.4855(11) 0.7616(8) 0.045(2) Uani 1 1 d . .
H9 H 0.6507 1.5472 0.8324 0.054 Uiso 1 1 calc R U
C10 C 0.5976(14) 1.5533(10) 0.6626(8) 0.043(2) Uani 1 1 d . .
H10 H 0.6833 1.6583 0.6679 0.052 Uiso 1 1 calc R U
C11 C 0.4924(12) 1.4669(9) 0.5559(7) 0.0310(18) Uani 1 1 d . .
C12 C 0.3649(14) 1.3117(11) 0.5557(8) 0.049(2) Uani 1 1 d . .
H12 H 0.2889 1.2484 0.4860 0.058 Uiso 1 1 calc R U
C13 C 0.3511(14) 1.2521(11) 0.6583(8) 0.047(2) Uani 1 1 d . .
H13 H 0.2642 1.1488 0.6559 0.056 Uiso 1 1 calc R U
O1 O 0.4046(8) 0.9610(6) 1.0890(5) 0.0381(14) Uani 1 1 d . .
O2 O 0.2269(9) 1.1078(7) 1.1356(6) 0.0469(17) Uani 1 1 d . .
O3 O -0.3168(8) 0.4823(7) 1.0274(5) 0.0402(15) Uani 1 1 d . .
O4 O -0.2676(8) 0.3027(7) 1.1431(5) 0.0397(14) Uani 1 1 d . .
O5 O 0.1306(10) 0.9632(9) 0.8088(8) 0.056(2) Uani 1 1 d D .
F1 F 0.0041(7) 0.6980(6) 1.0212(4) 0.0432(12) Uani 1 1 d . .
F2 F -0.0812(9) 0.4804(7) 1.3641(5) 0.0632(17) Uani 1 1 d . .
F3 F 0.1963(10) 0.7444(8) 1.4884(5) 0.077(2) Uani 1 1 d . .
F4 F 0.3749(8) 0.9886(6) 1.3810(5) 0.0589(16) Uani 1 1 d . .
H5A H 0.028(17) 0.940(15) 0.819(11) 0.071 Uiso 1 1 d . U
H5B H 0.054(14) 0.931(14) 0.745(5) 0.071 Uiso 1 1 d D U
N1 N 0.4579(11) 1.3370(9) 0.7618(6) 0.0401(18) Uani 1 1 d . .
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'
F F 0.0171 0.0103 '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
O1 Pb1 O3 97.54(19) 2_677 1_665
O1 Pb1 N1 83.5(2) 2_677 .
O3 Pb1 N1 76.4(2) 1_665 .
O1 Pb1 O1 67.7(2) 2_677 .
O3 Pb1 O1 119.25(19) 1_665 .
N1 Pb1 O1 148.13(19) . .
O1 Pb1 O4 76.41(19) 2_677 1_665
O3 Pb1 O4 48.62(18) 1_665 1_665
N1 Pb1 O4 116.6(2) . 1_665
O1 Pb1 O4 70.74(17) . 1_665
C2 C1 C6 115.9(7) . .
C2 C1 C7 121.1(7) . .
C6 C1 C7 123.0(7) . .
F1 C2 C1 115.9(6) . .
F1 C2 C3 118.8(7) . .
C1 C2 C3 125.1(7) . .
C4 C3 C2 114.9(7) . .
C4 C3 C8 122.8(7) . .
C2 C3 C8 122.1(7) . .
F2 C4 C5 117.0(8) . .
F2 C4 C3 120.4(8) . .
C5 C4 C3 122.6(8) . .
F3 C5 C6 120.2(8) . .
F3 C5 C4 120.5(8) . .
C6 C5 C4 119.3(8) . .
C5 C6 F4 119.5(8) . .
C5 C6 C1 122.2(8) . .
F4 C6 C1 118.3(7) . .
O1 C7 O2 125.5(7) . .
O1 C7 C1 118.5(6) . .
O2 C7 C1 116.0(7) . .
O4 C8 O3 122.2(7) . .
O4 C8 C3 121.7(8) . .
O3 C8 C3 116.1(7) . .
N1 C9 C10 123.7(9) . .
N1 C9 H9 118.1 . .
C10 C9 H9 118.1 . .
C11 C10 C9 120.4(8) . .
C11 C10 H10 119.8 . .
C9 C10 H10 119.8 . .
C10 C11 C12 116.1(7) . .
C10 C11 C11 123.3(9) . 2_686
C12 C11 C11 120.5(9) . 2_686
C13 C12 C11 120.3(8) . .
C13 C12 H12 119.8 . .
C11 C12 H12 119.8 . .
N1 C13 C12 122.7(8) . .
N1 C13 H13 118.6 . .
C12 C13 H13 118.6 . .
C7 O1 Pb1 149.0(5) . 2_677
C7 O1 Pb1 97.4(5) . .
Pb1 O1 Pb1 112.3(2) 2_677 .
C8 O3 Pb1 99.6(5) . 1_445
C8 O4 Pb1 89.3(5) . 1_445
H5A O5 H5B 72(10) . .
C9 N1 C13 116.7(8) . .
C9 N1 Pb1 121.8(6) . .
C13 N1 Pb1 121.4(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.437(6) 2_677
Pb1 O3 2.495(5) 1_665
Pb1 N1 2.708(7) .
Pb1 O1 2.717(5) .
Pb1 O4 2.738(6) 1_665
C1 C2 1.362(11) .
C1 C6 1.388(11) .
C1 C7 1.514(10) .
C2 F1 1.350(8) .
C2 C3 1.408(10) .
C3 C4 1.373(12) .
C3 C8 1.507(11) .
C4 F2 1.343(9) .
C4 C5 1.372(13) .
C5 F3 1.357(10) .
C5 C6 1.360(12) .
C6 F4 1.363(9) .
C7 O1 1.246(9) .
C7 O2 1.256(9) .
C8 O4 1.209(9) .
C8 O3 1.265(10) .
C9 N1 1.327(11) .
C9 C10 1.374(12) .
C9 H9 0.9300 .
C10 C11 1.373(11) .
C10 H10 0.9300 .
C11 C12 1.395(12) .
C11 C11 1.504(15) 2_686
C12 C13 1.375(12) .
C12 H12 0.9300 .
C13 N1 1.344(11) .
C13 H13 0.9300 .
O1 Pb1 2.437(6) 2_677
O3 Pb1 2.495(5) 1_445
O4 Pb1 2.738(6) 1_445
O5 H5A 0.80(11) .
O5 H5B 0.82(2) .
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
C6 C1 C2 F1 178.2(7) . .
C7 C1 C2 F1 1.6(11) . .
C6 C1 C2 C3 2.1(12) . .
C7 C1 C2 C3 -174.5(7) . .
F1 C2 C3 C4 -179.8(7) . .
C1 C2 C3 C4 -3.8(12) . .
F1 C2 C3 C8 -5.9(11) . .
C1 C2 C3 C8 170.1(7) . .
C2 C3 C4 F2 -179.9(8) . .
C8 C3 C4 F2 6.2(13) . .
C2 C3 C4 C5 3.1(13) . .
C8 C3 C4 C5 -170.8(8) . .
F2 C4 C5 F3 1.1(14) . .
C3 C4 C5 F3 178.1(9) . .
F2 C4 C5 C6 -178.0(8) . .
C3 C4 C5 C6 -0.9(14) . .
F3 C5 C6 F4 -0.2(14) . .
C4 C5 C6 F4 178.9(8) . .
F3 C5 C6 C1 179.9(8) . .
C4 C5 C6 C1 -1.0(14) . .
C2 C1 C6 C5 0.5(13) . .
C7 C1 C6 C5 177.0(8) . .
C2 C1 C6 F4 -179.4(7) . .
C7 C1 C6 F4 -2.9(12) . .
C2 C1 C7 O1 -80.0(10) . .
C6 C1 C7 O1 103.7(9) . .
C2 C1 C7 O2 99.8(9) . .
C6 C1 C7 O2 -76.6(11) . .
C4 C3 C8 O4 -37.7(12) . .
C2 C3 C8 O4 148.9(8) . .
C4 C3 C8 O3 144.5(8) . .
C2 C3 C8 O3 -29.0(11) . .
N1 C9 C10 C11 -0.2(15) . .
C9 C10 C11 C12 1.1(14) . .
C9 C10 C11 C11 -180.0(10) . 2_686
C10 C11 C12 C13 -0.8(14) . .
C11 C11 C12 C13 -179.7(10) 2_686 .
C11 C12 C13 N1 -0.6(16) . .
O2 C7 O1 Pb1 -176.6(7) . 2_677
C1 C7 O1 Pb1 3.2(15) . 2_677
O2 C7 O1 Pb1 -13.1(9) . .
C1 C7 O1 Pb1 166.6(6) . .
O4 C8 O3 Pb1 5.3(9) . 1_445
C3 C8 O3 Pb1 -176.9(6) . 1_445
O3 C8 O4 Pb1 -4.7(8) . 1_445
C3 C8 O4 Pb1 177.6(7) . 1_445
C10 C9 N1 C13 -1.1(14) . .
C10 C9 N1 Pb1 -177.8(7) . .
C12 C13 N1 C9 1.5(14) . .
C12 C13 N1 Pb1 178.2(8) . .
