#------------------------------------------------------------------------------
#$Date: 2016-03-26 04:00:09 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180205 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/99/7109945.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_7109945
loop_
_publ_author_name
'Xue-Li Cao'
'Chun-Li Hu'
'Xiang Xu'
'Fang Kong'
'Jiang-Gao Mao'
_publ_section_title
;
 Pb2TiOF(SeO3)2Cl and Pb2NbO2(SeO3)2Cl: small changes in structure induced
 a very large SHG enhancement
;
_journal_name_full               Chem.Commun.
_journal_page_first              9965
_journal_paper_doi               10.1039/c3cc45747h
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'Cl F O7 Pb2 Se2 Ti'
_chemical_formula_weight         786.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.191(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.2863(5)
_cell_length_b                   5.3781(2)
_cell_length_c                   10.7167(6)
_cell_measurement_reflns_used    2489
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.6146
_cell_measurement_theta_min      3.7810
_cell_volume                     445.29(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2899
_diffrn_reflns_theta_full        25.67
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         3.87
_exptl_absorpt_coefficient_mu    47.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49186
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    5.867
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rodlike
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.005
_refine_diff_density_min         -1.991
_refine_diff_density_rms         0.307
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(13)
_refine_ls_extinction_coef       0.0134(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1603
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0446P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                1562
_reflns_number_total             1603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc45747h.cif
_cod_data_source_block           Pb2TiOF(SeO3)Cl
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7109945
loop_
_symmetry_equiv_pos_as_xyz
'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 0.83133(6) 0.94026(12) 0.81259(5) 0.0184(2) Uani 1 1 d .
Pb2 Pb 0.29011(6) 0.98169(8) 0.50628(5) 0.01505(18) Uani 1 1 d .
Ti1 Ti 0.6529(2) 0.4764(5) 1.0432(2) 0.0075(4) Uani 1 1 d .
Se1 Se 1.12565(14) 0.4756(3) 0.80839(11) 0.0087(3) Uani 1 1 d .
Se2 Se 0.50901(14) 0.4851(3) 0.72164(11) 0.0097(3) Uani 1 1 d .
Cl1 Cl 0.8781(4) 1.0011(7) 0.5494(4) 0.0214(7) Uani 1 1 d .
O1 O 1.1665(11) 0.7003(18) 0.9305(10) 0.011(2) Uani 1 1 d .
O2 O 1.1232(13) 0.2121(19) 0.8965(11) 0.015(2) Uani 1 1 d U
O3 O 0.9120(11) 0.5288(18) 0.7333(9) 0.015(2) Uani 1 1 d .
O4 O 0.5591(13) 0.711(2) 0.6300(13) 0.016(2) Uani 1 1 d .
O5 O 0.5786(15) 0.234(2) 0.6621(12) 0.020(3) Uani 1 1 d .
O6 O 0.6761(12) 0.545(2) 0.8686(10) 0.019(2) Uani 1 1 d .
O7 O 0.4726(12) 0.2795(17) 0.9675(9) 0.013(2) Uani 1 1 d .
F1 F 0.6780(10) 0.432(2) 1.2241(8) 0.0230(19) 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
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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
O3 Pb1 O5 124.0(3) . 1_565
O3 Pb1 O6 65.7(3) . .
O5 Pb1 O6 105.8(3) 1_565 .
O3 Pb1 O2 105.8(3) . 1_565
O5 Pb1 O2 107.3(3) 1_565 1_565
O6 Pb1 O2 143.9(3) . 1_565
O3 Pb1 O4 67.1(3) . .
O5 Pb1 O4 63.9(3) 1_565 .
O6 Pb1 O4 56.8(3) . .
O2 Pb1 O4 155.3(3) 1_565 .
O3 Pb1 O1 55.5(3) . .
O5 Pb1 O1 161.7(3) 1_565 .
O6 Pb1 O1 90.7(3) . .
O2 Pb1 O1 59.5(3) 1_565 .
O4 Pb1 O1 122.1(3) . .
O3 Pb1 Cl1 69.0(2) . .
O5 Pb1 Cl1 72.9(3) 1_565 .
O6 Pb1 Cl1 122.4(2) . .
O2 Pb1 Cl1 81.3(2) 1_565 .
O4 Pb1 Cl1 74.1(3) . .
O1 Pb1 Cl1 91.7(2) . .
O3 Pb2 O4 69.6(3) 2_656 2_656
O3 Pb2 O4 135.2(4) 2_656 .
O4 Pb2 O4 93.2(3) 2_656 .
O3 Pb2 O5 133.3(3) 2_656 1_565
O4 Pb2 O5 67.0(3) 2_656 1_565
O4 Pb2 O5 64.2(3) . 1_565
O3 Pb2 O5 69.9(3) 2_656 2_656
O4 Pb2 O5 58.0(3) 2_656 2_656
O4 Pb2 O5 66.0(4) . 2_656
O5 Pb2 O5 100.1(2) 1_565 2_656
O3 Pb2 F1 146.7(2) 2_656 2_657
O4 Pb2 F1 138.4(3) 2_656 2_657
O4 Pb2 F1 71.2(3) . 2_657
O5 Pb2 F1 71.5(3) 1_565 2_657
O5 Pb2 F1 135.3(3) 2_656 2_657
O3 Pb2 Cl1 77.7(2) 2_656 2_646
O4 Pb2 Cl1 127.7(3) 2_656 2_646
O4 Pb2 Cl1 82.2(3) . 2_646
O5 Pb2 Cl1 145.0(3) 1_565 2_646
O5 Pb2 Cl1 73.0(3) 2_656 2_646
F1 Pb2 Cl1 89.2(2) 2_657 2_646
O3 Pb2 Cl1 67.9(2) 2_656 2_656
O4 Pb2 Cl1 74.5(2) 2_656 2_656
O4 Pb2 Cl1 148.6(3) . 2_656
O5 Pb2 Cl1 84.5(3) 1_565 2_656
O5 Pb2 Cl1 124.6(2) 2_656 2_656
F1 Pb2 Cl1 98.8(2) 2_657 2_656
Cl1 Pb2 Cl1 128.25(12) 2_646 2_656
O7 Ti1 F1 99.0(4) . .
O7 Ti1 O7 97.58(16) . 2_657
F1 Ti1 O7 91.4(4) . 2_657
O7 Ti1 O6 91.9(4) . .
F1 Ti1 O6 168.3(4) . .
O7 Ti1 O6 91.2(4) 2_657 .
O7 Ti1 O1 94.7(4) . 2_747
F1 Ti1 O1 87.9(4) . 2_747
O7 Ti1 O1 167.6(4) 2_657 2_747
O6 Ti1 O1 87.2(4) . 2_747
O7 Ti1 O2 170.5(4) . 2_757
F1 Ti1 O2 90.2(4) . 2_757
O7 Ti1 O2 84.6(4) 2_657 2_757
O6 Ti1 O2 78.8(4) . 2_757
O1 Ti1 O2 83.0(4) 2_747 2_757
O3 Se1 O2 100.7(5) . .
O3 Se1 O1 97.4(4) . .
O2 Se1 O1 101.6(5) . .
O5 Se2 O4 99.6(5) . .
O5 Se2 O6 103.1(6) . .
O4 Se2 O6 96.3(5) . .
Pb2 Cl1 Pb1 94.30(10) 2_656 .
Pb2 Cl1 Pb2 128.25(12) 2_656 2_646
Pb1 Cl1 Pb2 83.12(9) . 2_646
Se1 O1 Ti1 123.0(5) . 2_757
Se1 O1 Pb1 95.0(4) . .
Ti1 O1 Pb1 105.9(4) 2_757 .
Se1 O2 Ti1 118.4(5) . 2_747
Se1 O2 Pb1 117.1(5) . 1_545
Ti1 O2 Pb1 110.8(4) 2_747 1_545
Se1 O3 Pb2 131.8(5) . 2_646
Se1 O3 Pb1 110.2(4) . .
Pb2 O3 Pb1 105.6(3) 2_646 .
Se2 O4 Pb2 104.9(5) . 2_646
Se2 O4 Pb2 110.6(4) . .
Pb2 O4 Pb2 119.1(5) 2_646 .
Se2 O4 Pb1 102.8(6) . .
Pb2 O4 Pb1 100.5(3) 2_646 .
Pb2 O4 Pb1 117.0(4) . .
Se2 O5 Pb1 123.4(6) . 1_545
Se2 O5 Pb2 106.6(5) . 1_545
Pb1 O5 Pb2 113.7(4) 1_545 1_545
Se2 O6 Ti1 120.7(5) . .
Se2 O6 Pb1 103.9(5) . .
Ti1 O6 Pb1 125.6(5) . .
Ti1 O7 Ti1 152.4(5) . 2_647
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O3 2.545(10) .
Pb1 O5 2.652(12) 1_565
Pb1 O6 2.661(11) .
Pb1 O2 2.688(10) 1_565
Pb1 O4 2.692(12) .
Pb1 O1 2.905(10) .
Pb1 Cl1 3.000(4) .
Pb2 O3 2.520(9) 2_656
Pb2 O4 2.556(12) 2_656
Pb2 O4 2.591(10) .
Pb2 O5 2.730(11) 1_565
Pb2 O5 2.764(11) 2_656
Pb2 F1 2.818(8) 2_657
Pb2 Cl1 2.895(4) 2_646
Pb2 Cl1 3.082(4) 2_656
Ti1 O7 1.770(9) .
Ti1 F1 1.889(8) .
Ti1 O7 1.915(9) 2_657
Ti1 O6 1.984(10) .
Ti1 O1 2.054(9) 2_747
Ti1 O2 2.145(10) 2_757
Se1 O3 1.683(9) .
Se1 O2 1.707(10) .
Se1 O1 1.722(10) .
Se2 O5 1.683(12) .
Se2 O4 1.705(11) .
Se2 O6 1.711(10) .
Cl1 Pb2 2.895(4) 2_656
Cl1 Pb2 3.082(4) 2_646
O1 Ti1 2.054(9) 2_757
O2 Ti1 2.145(10) 2_747
O2 Pb1 2.688(10) 1_545
O3 Pb2 2.520(9) 2_646
O4 Pb2 2.556(12) 2_646
O5 Pb1 2.652(12) 1_545
O5 Pb2 2.730(11) 1_545
O7 Ti1 1.915(9) 2_647
