#------------------------------------------------------------------------------
#$Date: 2019-11-10 18:59:29 +0200 (Sun, 10 Nov 2019) $
#$Revision: 225973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/58/4515881.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_4515881
loop_
_publ_author_name
'Roy, Sourav'
'Halder, Soumi'
'Drew, Michael G. B.'
'Ray, Partha Pratim'
'Chattopadhyay, Shouvik'
_publ_section_title
;
 Fabrication of an Active Electronic Device Using a Hetero-bimetallic
 Coordination Polymer.
;
_journal_issue                   10
_journal_name_full               'ACS omega'
_journal_page_first              12788
_journal_page_last               12796
_journal_paper_doi               10.1021/acsomega.8b02025
_journal_volume                  3
_journal_year                    2018
_chemical_formula_sum            'C21 H22 N4 Ni O5 Pb S2'
_chemical_formula_weight         740.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 105.941(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3716(6)
_cell_length_b                   9.6865(3)
_cell_length_c                   20.7826(13)
_cell_measurement_reflns_used    15388
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      3.425
_cell_volume                     2394.8(2)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material
'SHELXL-2016/6, PLATON, WINGX (Ferrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       'Oxford Diffaction X-Calibor System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15388
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         3.425
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_exptl_absorpt_coefficient_mu    8.023
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.838
_refine_diff_density_min         -2.115
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         6823
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0538
_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)+(0.0309P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5172
_reflns_number_total             6823
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ao8b02025_si_001.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4515881
_shelx_shelxl_version_number     2016/6
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
_atom_site_refinement_flags_occupancy
Pb1 Pb 0.09233(2) 0.06273(2) 0.20392(2) 0.02720(8) Uani 1 1 d D . .
Ni1 Ni -0.06458(6) -0.23731(7) 0.17055(4) 0.02025(17) Uani 1 1 d . . .
N1 N 0.4232(4) 0.1321(5) 0.2977(3) 0.0309(13) Uani 1 1 d . . .
C1 C 0.3667(5) 0.0352(6) 0.2864(3) 0.0312(16) Uani 1 1 d . . .
S1 S 0.28395(16) -0.10039(17) 0.27026(12) 0.0497(6) Uani 1 1 d . . .
O11 O 0.0261(3) -0.1119(4) 0.1261(2) 0.0236(9) Uani 1 1 d . . .
C12 C 0.0571(5) -0.1371(6) 0.0716(3) 0.0237(13) Uani 1 1 d . . .
C13 C 0.1420(5) -0.0556(6) 0.0554(4) 0.0320(16) Uani 1 1 d . . .
C14 C 0.1746(6) -0.0752(6) -0.0006(4) 0.0380(17) Uani 1 1 d . . .
H14 H 0.231149 -0.020214 -0.008642 0.046 Uiso 1 1 calc R U .
C15 C 0.1244(7) -0.1773(7) -0.0470(4) 0.0442(19) Uani 1 1 d . . .
H15 H 0.144821 -0.189005 -0.086478 0.053 Uiso 1 1 calc R U .
C16 C 0.0440(6) -0.2597(7) -0.0320(3) 0.0349(16) Uani 1 1 d . . .
H16 H 0.011447 -0.329465 -0.061783 0.042 Uiso 1 1 calc R U .
C17 C 0.0091(5) -0.2428(6) 0.0261(3) 0.0260(14) Uani 1 1 d . . .
C18 C -0.0777(5) -0.3359(6) 0.0341(3) 0.0280(15) Uani 1 1 d . . .
H18 H -0.108495 -0.394027 -0.001856 0.034 Uiso 1 1 calc R U .
N19 N -0.1174(4) -0.3482(5) 0.0848(3) 0.0233(11) Uani 1 1 d . . .
C20 C -0.2067(6) -0.4510(6) 0.0787(4) 0.0349(16) Uani 1 1 d . . .
H20A H -0.207369 -0.512532 0.041806 0.042 Uiso 1 1 calc R U .
H20B H -0.278767 -0.404382 0.068662 0.042 Uiso 1 1 calc R U .
C21 C -0.1909(6) -0.5350(6) 0.1421(4) 0.0405(19) Uani 1 1 d . . .
H21A H -0.236815 -0.617530 0.131672 0.049 Uiso 1 1 calc R U .
H21B H -0.112983 -0.564127 0.157432 0.049 Uiso 1 1 calc R U .
C22 C -0.2206(7) -0.4599(7) 0.1982(4) 0.0432(19) Uani 1 1 d . . .
H22A H -0.294944 -0.419969 0.181241 0.052 Uiso 1 1 calc R U .
H22B H -0.223862 -0.525950 0.232661 0.052 Uiso 1 1 calc R U .
N23 N -0.1404(4) -0.3489(5) 0.2285(3) 0.0284(13) Uani 1 1 d . . .
C24 C -0.1202(5) -0.3341(6) 0.2908(3) 0.0283(15) Uani 1 1 d . . .
H24 H -0.154242 -0.398101 0.312290 0.034 Uiso 1 1 calc R U .
C25 C -0.0504(5) -0.2302(6) 0.3342(3) 0.0221(13) Uani 1 1 d . . .
C26 C -0.0384(5) -0.2447(7) 0.4027(3) 0.0321(16) Uani 1 1 d . . .
H26 H -0.071819 -0.319594 0.417678 0.038 Uiso 1 1 calc R U .
C27 C 0.0211(6) -0.1515(8) 0.4484(4) 0.0400(18) Uani 1 1 d . . .
H27 H 0.028911 -0.163219 0.493837 0.048 Uiso 1 1 calc R U .
C28 C 0.0704(6) -0.0373(7) 0.4250(4) 0.0391(18) Uani 1 1 d . . .
H28 H 0.109973 0.027929 0.455277 0.047 Uiso 1 1 calc R U .
C29 C 0.0605(5) -0.0221(6) 0.3593(4) 0.0300(16) Uani 1 1 d . . .
C30 C 0.0016(5) -0.1197(6) 0.3107(3) 0.0220(13) Uani 1 1 d . . .
O31 O -0.0032(3) -0.1025(4) 0.2469(2) 0.0278(10) Uani 1 1 d . . .
O131 O 0.1858(4) 0.0446(4) 0.1035(3) 0.0344(11) Uani 1 1 d . . .
C132 C 0.2846(6) 0.1169(7) 0.0983(4) 0.045(2) Uani 1 1 d . . .
H13A H 0.341859 0.051418 0.096404 0.068 Uiso 1 1 calc R U .
H13B H 0.311391 0.175541 0.136578 0.068 Uiso 1 1 calc R U .
H13C H 0.266355 0.172042 0.058343 0.068 Uiso 1 1 calc R U .
O291 O 0.1044(4) 0.0868(4) 0.3325(3) 0.0364(12) Uani 1 1 d . . .
C292 C 0.1857(7) 0.1709(8) 0.3786(4) 0.059(2) Uani 1 1 d . . .
H29A H 0.151640 0.211618 0.410379 0.088 Uiso 1 1 calc R U .
H29B H 0.211391 0.242529 0.354477 0.088 Uiso 1 1 calc R U .
H29C H 0.248243 0.114809 0.401750 0.088 Uiso 1 1 calc R U .
C2 C -0.3064(6) -0.1336(7) 0.1314(4) 0.051(2) Uani 1 1 d . . .
N2 N -0.2145(5) -0.1138(6) 0.1382(3) 0.0343(14) Uani 1 1 d . . .
S21 S -0.4371(2) -0.1714(3) 0.13349(19) 0.0452(11) Uani 0.725(7) 1 d . . P
S22 S -0.4370(7) -0.1096(10) 0.0739(7) 0.077(5) Uani 0.275(7) 1 d . . P
O1 O -0.1058(5) 0.1680(6) 0.2121(4) 0.076(2) Uani 1 1 d D . .
H1 H -0.085(2) 0.209(7) 0.252(2) 0.091 Uiso 1 1 d D U .
H2 H -0.140(3) 0.090(3) 0.219(4) 0.091 Uiso 1 1 d D 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'
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
O31 Pb1 O11 69.24(15) . .
O31 Pb1 O291 64.13(14) . .
O11 Pb1 O291 132.65(13) . .
O31 Pb1 O131 129.61(14) . .
O11 Pb1 O131 63.37(13) . .
O291 Pb1 O131 152.11(14) . .
O31 Pb1 O1 70.60(16) . .
O11 Pb1 O1 99.55(18) . .
O291 Pb1 O1 72.77(18) . .
O131 Pb1 O1 132.28(18) . .
O31 Pb1 S1 82.85(11) . .
O11 Pb1 S1 91.17(10) . .
O291 Pb1 S1 75.69(11) . .
O131 Pb1 S1 81.99(11) . .
O1 Pb1 S1 145.27(15) . .
N19 Ni1 N23 98.6(2) . .
N19 Ni1 O31 170.45(19) . .
N23 Ni1 O31 90.7(2) . .
N19 Ni1 O11 90.12(19) . .
N23 Ni1 O11 171.0(2) . .
O31 Ni1 O11 80.62(17) . .
N19 Ni1 N1 89.8(2) . 2_545
N23 Ni1 N1 88.5(2) . 2_545
O31 Ni1 N1 92.36(19) . 2_545
O11 Ni1 N1 89.22(18) . 2_545
N19 Ni1 N2 88.7(2) . .
N23 Ni1 N2 89.0(2) . .
O31 Ni1 N2 89.5(2) . .
O11 Ni1 N2 93.53(18) . .
N1 Ni1 N2 176.9(2) 2_545 .
C1 N1 Ni1 162.3(5) . 2
N1 C1 S1 178.6(6) . .
C1 S1 Pb1 92.5(2) . .
C12 O11 Ni1 127.3(4) . .
C12 O11 Pb1 127.1(3) . .
Ni1 O11 Pb1 104.49(19) . .
O11 C12 C17 123.0(6) . .
O11 C12 C13 120.5(6) . .
C17 C12 C13 116.5(6) . .
C14 C13 O131 124.7(6) . .
C14 C13 C12 122.7(6) . .
O131 C13 C12 112.6(6) . .
C13 C14 C15 120.8(7) . .
C13 C14 H14 119.6 . .
C15 C14 H14 119.6 . .
C16 C15 C14 117.7(7) . .
C16 C15 H15 121.1 . .
C14 C15 H15 121.1 . .
C15 C16 C17 122.7(7) . .
C15 C16 H16 118.6 . .
C17 C16 H16 118.6 . .
C16 C17 C12 119.4(6) . .
C16 C17 C18 116.2(6) . .
C12 C17 C18 124.4(6) . .
N19 C18 C17 128.0(6) . .
N19 C18 H18 116.0 . .
C17 C18 H18 116.0 . .
C18 N19 C20 116.2(5) . .
C18 N19 Ni1 124.6(4) . .
C20 N19 Ni1 119.2(4) . .
N19 C20 C21 112.1(5) . .
N19 C20 H20A 109.2 . .
C21 C20 H20A 109.2 . .
N19 C20 H20B 109.2 . .
C21 C20 H20B 109.2 . .
H20A C20 H20B 107.9 . .
C22 C21 C20 114.4(6) . .
C22 C21 H21A 108.7 . .
C20 C21 H21A 108.7 . .
C22 C21 H21B 108.7 . .
C20 C21 H21B 108.7 . .
H21A C21 H21B 107.6 . .
N23 C22 C21 113.8(6) . .
N23 C22 H22A 108.8 . .
C21 C22 H22A 108.8 . .
N23 C22 H22B 108.8 . .
C21 C22 H22B 108.8 . .
H22A C22 H22B 107.7 . .
C24 N23 C22 116.2(6) . .
C24 N23 Ni1 123.8(4) . .
C22 N23 Ni1 119.9(5) . .
N23 C24 C25 129.0(6) . .
N23 C24 H24 115.5 . .
C25 C24 H24 115.5 . .
C26 C25 C30 120.0(6) . .
C26 C25 C24 116.0(6) . .
C30 C25 C24 123.9(6) . .
C27 C26 C25 121.8(7) . .
C27 C26 H26 119.1 . .
C25 C26 H26 119.1 . .
C26 C27 C28 118.6(7) . .
C26 C27 H27 120.7 . .
C28 C27 H27 120.7 . .
C29 C28 C27 120.5(6) . .
C29 C28 H28 119.8 . .
C27 C28 H28 119.8 . .
C28 C29 O291 124.0(6) . .
C28 C29 C30 122.1(6) . .
O291 C29 C30 113.8(6) . .
O31 C30 C25 123.1(5) . .
O31 C30 C29 120.0(5) . .
C25 C30 C29 116.9(6) . .
C30 O31 Ni1 127.3(3) . .
C30 O31 Pb1 126.0(3) . .
Ni1 O31 Pb1 105.3(2) . .
C13 O131 C132 117.2(6) . .
C13 O131 Pb1 116.2(4) . .
C132 O131 Pb1 126.1(4) . .
O131 C132 H13A 109.5 . .
O131 C132 H13B 109.5 . .
H13A C132 H13B 109.5 . .
O131 C132 H13C 109.5 . .
H13A C132 H13C 109.5 . .
H13B C132 H13C 109.5 . .
C29 O291 C292 116.6(6) . .
C29 O291 Pb1 115.0(4) . .
C292 O291 Pb1 124.0(5) . .
O291 C292 H29A 109.5 . .
O291 C292 H29B 109.5 . .
H29A C292 H29B 109.5 . .
O291 C292 H29C 109.5 . .
H29A C292 H29C 109.5 . .
H29B C292 H29C 109.5 . .
N2 C2 S21 171.1(9) . .
N2 C2 S22 141.4(10) . .
S21 C2 S22 47.5(5) . .
C2 N2 Ni1 134.4(6) . .
S22 S21 C2 69.0(5) . .
S21 S22 C2 63.6(5) . .
Pb1 O1 H1 101.3(17) . .
Pb1 O1 H2 99.8(16) . .
H1 O1 H2 105(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O31 2.310(4) .
Pb1 O11 2.328(4) .
Pb1 O291 2.645(5) .
Pb1 O131 2.656(5) .
Pb1 O1 2.703(7) .
Pb1 S1 2.867(2) .
Ni1 N19 2.029(5) .
Ni1 N23 2.030(5) .
Ni1 O31 2.034(4) .
Ni1 O11 2.040(4) .
Ni1 N1 2.112(5) 2_545
Ni1 N2 2.154(6) .
N1 C1 1.155(8) .
C1 S1 1.642(7) .
O11 C12 1.315(7) .
C12 C17 1.409(8) .
C12 C13 1.426(9) .
C13 C14 1.346(10) .
C13 O131 1.392(8) .
C14 C15 1.401(10) .
C14 H14 0.9300 .
C15 C16 1.376(10) .
C15 H15 0.9300 .
C16 C17 1.399(9) .
C16 H16 0.9300 .
C17 C18 1.447(8) .
C18 N19 1.285(8) .
C18 H18 0.9300 .
N19 C20 1.466(7) .
C20 C21 1.515(10) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C21 C22 1.502(10) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 N23 1.482(8) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
N23 C24 1.256(8) .
C24 C25 1.464(8) .
C24 H24 0.9300 .
C25 C26 1.397(9) .
C25 C30 1.405(8) .
C26 C27 1.369(9) .
C26 H26 0.9300 .
C27 C28 1.413(10) .
C27 H27 0.9300 .
C28 C29 1.346(10) .
C28 H28 0.9300 .
C29 O291 1.372(8) .
C29 C30 1.428(8) .
C30 O31 1.321(7) .
O131 C132 1.437(7) .
C132 H13A 0.9600 .
C132 H13B 0.9600 .
C132 H13C 0.9600 .
O291 C292 1.436(8) .
C292 H29A 0.9600 .
C292 H29B 0.9600 .
C292 H29C 0.9600 .
C2 N2 1.123(8) .
C2 S21 1.670(8) .
C2 S22 1.741(11) .
S21 S22 1.375(14) .
O1 H1 0.88(2) .
O1 H2 0.90(2) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 S21 0.88(2) 2.60(2) 3.473(8) 170(3) 2_455
O1 H2 O31 0.90(2) 2.48(3) 2.914(7) 110(2) .
O1 H2 N2 0.90(2) 2.59(6) 3.237(9) 130(6) .
