#------------------------------------------------------------------------------
#$Date: 2025-03-04 21:58:09 +0200 (Tue, 04 Mar 2025) $
#$Revision: 298232 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/74/7717495.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_7717495
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 O2 Pb'
_chemical_formula_sum            'C2 N2 O2 Pb'
_chemical_formula_weight         291.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5689(18)
_cell_length_b                   3.9410(9)
_cell_length_c                   11.660(3)
_cell_measurement_reflns_used    3543
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.10
_cell_measurement_theta_min      1.68
_cell_volume                     393.76(16)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
 291 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  0.0993
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6464
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.906
_diffrn_reflns_theta_min         2.950
_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    42.695
_exptl_absorpt_correction_T_max  0.0010
_exptl_absorpt_correction_T_min  0.0001
_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    4.913
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.712
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.482
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0415
_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)+(0.0610P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.0970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                517
_reflns_number_total             760
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02830a2.cif
_cod_data_source_block           Pb_(OCN)2
_cod_depositor_comments
'Adding full bibliography for 7717495--7717498.cif.'
_cod_original_cell_volume        393.74(17)
_cod_database_code               7717495
_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   0.100
_shelx_estimated_absorpt_t_min   0.072
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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 0.18174(7) 0.750000 0.40656(5) 0.02332(19) Uani 1 2 d S T P . .
O1 O 0.2333(13) 0.750000 0.7443(10) 0.028(2) Uani 1 2 d S T P . .
O2 O 0.4959(12) 0.250000 0.6678(10) 0.026(2) Uani 1 2 d S T P . .
N1 N 0.0308(14) 0.750000 0.6007(11) 0.022(2) Uani 1 2 d S T P . .
N2 N 0.3106(16) 0.250000 0.5151(12) 0.029(3) Uani 1 2 d S T P . .
C1 C 0.1290(18) 0.750000 0.6743(13) 0.019(3) Uani 1 2 d S T P . .
C2 C 0.4042(17) 0.250000 0.5906(15) 0.026(3) Uani 1 2 d S T P . .
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'
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
_geom_angle_publ_flag
N1 Pb1 N1 72.0(3) . 5_576 ?
N1 Pb1 N1 94.4(4) 5_566 5_576 ?
N1 Pb1 N1 72.0(4) . 5_566 ?
N2 Pb1 N1 75.3(3) 1_565 5_576 ?
N2 Pb1 N1 75.3(3) . 5_566 ?
N2 Pb1 N1 77.7(3) . . ?
N2 Pb1 N1 77.7(3) 1_565 . ?
N2 Pb1 N1 149.7(4) 1_565 5_566 ?
N2 Pb1 N1 149.7(4) . 5_576 ?
N2 Pb1 N2 99.1(5) 1_565 . ?
Pb1 N1 Pb1 108.0(3) . 5_566 ?
Pb1 N1 Pb1 94.5(4) 5_566 5_576 ?
Pb1 N1 Pb1 108.0(3) . 5_576 ?
C1 N1 Pb1 105.8(10) . . ?
C1 N1 Pb1 119.8(6) . 5_566 ?
C1 N1 Pb1 119.8(6) . 5_576 ?
Pb1 N2 Pb1 99.1(5) 1_545 . ?
C2 N2 Pb1 130.4(2) . . ?
C2 N2 Pb1 130.4(2) . 1_545 ?
N1 C1 O1 176.8(17) . . ?
N2 C2 O2 178.8(17) . . ?
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 N1 2.607(13) . ?
Pb1 N1 2.685(8) 5_576 ?
Pb1 N1 2.685(8) 5_566 ?
Pb1 N2 2.589(9) . ?
Pb1 N2 2.589(9) 1_565 ?
O1 C1 1.210(18) . ?
O2 C2 1.195(19) . ?
N1 C1 1.203(19) . ?
N2 C2 1.19(2) . ?
