#------------------------------------------------------------------------------
#$Date: 2025-03-04 21:58:09 +0200 (Tue, 04 Mar 2025) $
#$Revision: 298232 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/74/7717496.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_7717496
loop_
_publ_author_name
'Shlyaykher, Alena'
'Živković, Aleksandar'
'Günther, Hennes'
'Barba, Anna Lea'
'de Leeuw, Nora H.'
'Tambornino, Frank'
_publ_section_title
;
 Synthesis, XRD and DFT studies on Pb[ChCN]₂ (Ch = O, S, Se)
 and Pb[SeCN][OH].
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              74
_journal_page_last               88
_journal_paper_doi               10.1039/d4dt02830a
_journal_volume                  54
_journal_year                    2024
_chemical_formula_moiety         'C2 N2 Pb S2'
_chemical_formula_sum            'C2 N2 Pb S2'
_chemical_formula_weight         323.35
_chemical_name_systematic        Pb(SCN)2
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_audit_creation_date             2022-09-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-09-13 deposited with the CCDC.	2024-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.734(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6128(9)
_cell_length_b                   6.5306(6)
_cell_length_c                   8.1913(7)
_cell_measurement_reflns_used    14096
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.01
_cell_measurement_theta_min      2.05
_cell_volume                     513.64(8)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.72.0.0 (STOE, 2018)
X-Area LANA 1.71.6.0 (STOE, 2017)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.81, Darmstadt 2018
;
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'imaging plate area detector'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
 540 frames, detector distance = 80 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_collimation    '0.5 mm, multiple pinhole'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_av_unetI/netI     0.0084
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5951
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.488
_diffrn_reflns_theta_min         4.245
_diffrn_source                   'sealed X-ray tube, 12 x 0.4 mm LF focus'
_diffrn_source_current           0.000
_diffrn_source_power             0.000
_diffrn_source_target            Mo
_diffrn_source_type              'STOE C-Tech Mo LFF X-Ray Tube'
_diffrn_source_voltage           0
_exptl_absorpt_coefficient_mu    33.507
_exptl_absorpt_correction_T_max  0.0003
_exptl_absorpt_correction_T_min  0.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.026
_refine_diff_density_min         -1.403
_refine_diff_density_rms         0.176
_refine_ls_extinction_coef       0.00137(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0130
_refine_ls_R_factor_gt           0.0124
_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)+(0.0219P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0303
_refine_ls_wR_factor_ref         0.0304
_reflns_Friedel_coverage         0.000
_reflns_number_gt                763
_reflns_number_total             786
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02830a2.cif
_cod_data_source_block           Pb_(SCN)2
_cod_depositor_comments
'Adding full bibliography for 7717495--7717498.cif.'
_cod_database_code               7717496
_shelx_shelxl_version_number     2018/3
_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_max   0.433
_shelx_estimated_absorpt_t_min   0.175
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.500000 1.38980(2) 0.250000 0.01488(7) Uani 1 2 d S T P . .
S1 S 0.70778(7) 1.06024(11) 0.32902(9) 0.01913(13) Uani 1 1 d . . . . .
N1 N 0.5568(3) 0.7269(4) 0.4464(3) 0.0179(4) Uani 1 1 d . . . . .
C1 C 0.6186(3) 0.8666(4) 0.3988(3) 0.0163(5) 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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0618
30 17 4 0.0728
16 13 30 0.0446
13 -14 30 0.0445
3 0 -5 0.0517
1 6 0 0.0995
1 1 30 0.0325
-4 -5 30 0.0407
-30 0 1 0.0526
-10 -6 1 0.0831
-16 -9 -30 0.0459
-17 11 -30 0.0449
-23 10 30 0.0688
-22 -5 30 0.0533
2 -30 1 0.0900
0 0 -1 0.0278
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
_geom_angle_publ_flag
S1 Pb1 S1 87.77(3) 2_655 . ?
S1 Pb1 S1 72.686(12) . 4_655 ?
S1 Pb1 S1 144.31(2) 2_655 4_655 ?
S1 Pb1 S1 72.686(12) 2_655 3_455 ?
S1 Pb1 S1 138.17(3) 4_655 3_455 ?
S1 Pb1 S1 144.31(2) . 3_455 ?
N1 Pb1 S1 109.64(5) 1_565 . ?
N1 Pb1 S1 121.28(5) 6_575 3_455 ?
N1 Pb1 S1 75.99(5) 5_676 . ?
N1 Pb1 S1 144.22(5) 2_665 . ?
N1 Pb1 S1 75.52(5) 1_565 3_455 ?
N1 Pb1 S1 75.99(5) 6_575 2_655 ?
N1 Pb1 S1 80.36(5) 6_575 . ?
N1 Pb1 S1 80.36(5) 5_676 2_655 ?
N1 Pb1 S1 71.56(5) 5_676 3_455 ?
N1 Pb1 S1 144.22(5) 1_565 2_655 ?
N1 Pb1 S1 71.45(5) 2_665 3_455 ?
N1 Pb1 S1 75.52(5) 2_665 4_655 ?
N1 Pb1 S1 109.64(5) 2_665 2_655 ?
N1 Pb1 S1 71.56(5) 6_575 4_655 ?
N1 Pb1 S1 121.28(5) 5_676 4_655 ?
N1 Pb1 S1 71.45(5) 1_565 4_655 ?
N1 Pb1 N1 74.34(8) 6_575 2_665 ?
N1 Pb1 N1 74.34(8) 5_676 1_565 ?
N1 Pb1 N1 136.25(7) 6_575 1_565 ?
N1 Pb1 N1 136.25(7) 5_676 2_665 ?
N1 Pb1 N1 74.51(10) 1_565 2_665 ?
N1 Pb1 N1 146.98(11) 6_575 5_676 ?
Pb1 S1 Pb1 144.31(2) . 3_545 ?
C1 S1 Pb1 106.69(10) . 3_545 ?
C1 S1 Pb1 105.96(10) . . ?
Pb1 N1 Pb1 105.66(8) 5_676 1_545 ?
C1 N1 Pb1 131.5(2) . 5_676 ?
C1 N1 Pb1 121.2(2) . 1_545 ?
N1 C1 S1 178.7(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 S1 2.9862(7) . ?
Pb1 S1 3.1180(7) 3_455 ?
Pb1 S1 3.1180(7) 4_655 ?
Pb1 S1 2.9862(7) 2_655 ?
Pb1 N1 2.682(2) 6_575 ?
Pb1 N1 2.766(2) 1_565 ?
Pb1 N1 2.766(2) 2_665 ?
Pb1 N1 2.682(2) 5_676 ?
S1 C1 1.645(3) . ?
N1 C1 1.166(4) . ?
