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#$Date: 2022-10-12 02:07:20 +0300 (Wed, 12 Oct 2022) $
#$Revision: 278539 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/14/7711466.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_7711466
loop_
_publ_author_name
'Popov, Georgi'
'Bačić, Goran'
'Van Dijck, Charlotte'
'Junkers, Laura S.'
'Weiß, Alexander'
'Mattinen, Miika'
'Vihervaara, Anton'
'Chundak, Mykhailo'
'Jalkanen, Pasi'
'Mizohata, Kenichiro'
'Leskelä, Markku'
'Masuda, Jason D.'
'Barry, Seán T'
'Ritala, Mikko'
'Kemell, Marianna'
_publ_section_title
;
 Atomic layer deposition of PbCl₂, PbBr₂ and mixed
 lead halide (Cl, Br, I) PbXₙY₂₋ₙ thin
 films.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15142
_journal_page_last               15157
_journal_paper_doi               10.1039/d2dt02216h
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C20 H48 N4 Pb2 Si2'
_chemical_formula_sum            'C20 H48 N4 Pb2 Si2'
_chemical_formula_weight         815.18
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-06-22 deposited with the CCDC.	2022-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.094(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.967(3)
_cell_length_b                   13.051(4)
_cell_length_c                   19.827(5)
_cell_measurement_reflns_used    4877
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      27.73
_cell_measurement_theta_min      2.55
_cell_volume                     2809.6(14)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      125.07
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17398
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.262
_diffrn_reflns_theta_min         2.075
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.067
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1142 before and 0.0476 after correction. The Ratio of minimum to maximum transmission is 0.7200. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         3623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0231
_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)+(0.0177P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0417
_refine_ls_wR_factor_ref         0.0446
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3041
_reflns_number_total             3623
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt02216h4.cif
_cod_data_source_block           2019_04_04_sb_gb421pb_0m_a
_cod_original_cell_volume        2809.6(13)
_cod_database_code               7711466
_shelx_shelxl_version_number     2014/7
_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   0.445
_shelx_estimated_absorpt_t_min   0.350
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_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
C1 C 0.2503(3) 0.4149(3) 0.32098(18) 0.0168(8) Uani 1 1 d . . . . .
N1 N 0.2907(3) 0.3545(2) 0.38294(14) 0.0139(6) Uani 1 1 d . . . . .
Pb1 Pb 0.25908(2) 0.38769(2) 0.48865(2) 0.01154(4) Uani 1 1 d . . . . .
Si1 Si 0.39213(9) 0.25575(7) 0.39792(5) 0.0138(2) Uani 1 1 d . . . . .
C2 C 0.3552(4) 0.4837(3) 0.3043(2) 0.0285(10) Uani 1 1 d . . . . .
H2A H 0.3789 0.5313 0.3421 0.043 Uiso 1 1 calc GR . . . .
H2B H 0.3276 0.5226 0.2627 0.043 Uiso 1 1 calc GR . . . .
H2C H 0.4261 0.4413 0.2975 0.043 Uiso 1 1 calc GR . . . .
N2 N 0.3943(3) 0.2489(2) 0.48763(15) 0.0118(6) Uani 1 1 d . . . . .
C3 C 0.2085(4) 0.3447(3) 0.25953(18) 0.0251(9) Uani 1 1 d . . . . .
H3A H 0.1797 0.3867 0.2195 0.038 Uiso 1 1 calc GR . . . .
H3B H 0.1415 0.3004 0.2699 0.038 Uiso 1 1 calc GR . . . .
H3C H 0.2780 0.3023 0.2501 0.038 Uiso 1 1 calc GR . . . .
C4 C 0.1423(4) 0.4835(3) 0.33300(19) 0.0243(9) Uani 1 1 d . . . . .
H4A H 0.0715 0.4408 0.3397 0.036 Uiso 1 1 calc GR . . . .
H4B H 0.1201 0.5281 0.2934 0.036 Uiso 1 1 calc GR . . . .
H4C H 0.1662 0.5256 0.3737 0.036 Uiso 1 1 calc GR . . . .
C5 C 0.5105(3) 0.2506(3) 0.53770(18) 0.0142(8) Uani 1 1 d . . . . .
C6 C 0.6000(3) 0.3337(3) 0.52268(19) 0.0220(9) Uani 1 1 d . . . . .
H6A H 0.6659 0.3401 0.5613 0.033 Uiso 1 1 calc GR . . . .
H6B H 0.5562 0.3990 0.5154 0.033 Uiso 1 1 calc GR . . . .
H6C H 0.6356 0.3154 0.4817 0.033 Uiso 1 1 calc GR . . . .
C7 C 0.4784(3) 0.2730(3) 0.60898(18) 0.0187(8) Uani 1 1 d . . . . .
H7A H 0.4477 0.3433 0.6106 0.028 Uiso 1 1 calc GR . . . .
H7B H 0.5522 0.2649 0.6427 0.028 Uiso 1 1 calc GR . . . .
H7C H 0.4148 0.2250 0.6193 0.028 Uiso 1 1 calc GR . . . .
C8 C 0.5734(4) 0.1461(3) 0.5377(2) 0.0227(9) Uani 1 1 d . . . . .
H8A H 0.5198 0.0936 0.5530 0.034 Uiso 1 1 calc GR . . . .
H8B H 0.6515 0.1479 0.5685 0.034 Uiso 1 1 calc GR . . . .
H8C H 0.5893 0.1299 0.4914 0.034 Uiso 1 1 calc GR . . . .
C9 C 0.3414(4) 0.1302(3) 0.35573(19) 0.0219(9) Uani 1 1 d . . . . .
H9A H 0.3940 0.0748 0.3767 0.033 Uiso 1 1 calc GR . . . .
H9B H 0.3483 0.1341 0.3070 0.033 Uiso 1 1 calc GR . . . .
H9C H 0.2557 0.1166 0.3615 0.033 Uiso 1 1 calc GR . . . .
C10 C 0.5427(4) 0.2762(3) 0.3641(2) 0.0234(9) Uani 1 1 d . . . . .
H10A H 0.5741 0.3449 0.3766 0.035 Uiso 1 1 calc GR . . . .
H10B H 0.5296 0.2694 0.3143 0.035 Uiso 1 1 calc GR . . . .
H10C H 0.6026 0.2248 0.3837 0.035 Uiso 1 1 calc GR . . . .
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'
Si Si 0.0817 0.0704 '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 C1 C2 110.3(3) . . ?
N1 C1 C3 111.2(3) . . ?
N1 C1 C4 109.3(3) . . ?
C2 C1 C3 109.1(3) . . ?
C4 C1 C2 108.1(3) . . ?
C4 C1 C3 108.7(3) . . ?
C1 N1 Pb1 128.0(2) . . ?
C1 N1 Si1 131.5(2) . . ?
Si1 N1 Pb1 99.70(13) . . ?
N1 Pb1 Pb1 86.70(8) . 7_556 ?
N1 Pb1 Si1 33.84(8) . . ?
N1 Pb1 N2 69.95(10) . . ?
N1 Pb1 N2 103.53(10) . 7_556 ?
Si1 Pb1 Pb1 63.11(2) . 7_556 ?
N2 Pb1 Pb1 44.08(7) . 7_556 ?
N2 Pb1 Pb1 39.91(6) 7_556 7_556 ?
N2 Pb1 Si1 36.12(7) . . ?
N2 Pb1 Si1 95.65(7) 7_556 . ?
N2 Pb1 N2 83.99(10) . 7_556 ?
N1 Si1 Pb1 46.46(10) . . ?
N1 Si1 N2 97.41(14) . . ?
N1 Si1 C9 115.84(17) . . ?
N1 Si1 C10 114.49(17) . . ?
N2 Si1 Pb1 50.98(9) . . ?
N2 Si1 C9 111.19(16) . . ?
N2 Si1 C10 118.29(16) . . ?
C9 Si1 Pb1 128.60(13) . . ?
C10 Si1 Pb1 130.82(13) . . ?
C10 Si1 C9 100.53(18) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Pb1 N2 Pb1 96.00(10) . 7_556 ?
Si1 N2 Pb1 107.74(13) . 7_556 ?
Si1 N2 Pb1 92.90(12) . . ?
C5 N2 Pb1 117.5(2) . . ?
C5 N2 Pb1 114.2(2) . 7_556 ?
C5 N2 Si1 123.5(2) . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C6 113.1(3) . . ?
N2 C5 C7 109.2(3) . . ?
N2 C5 C8 109.1(3) . . ?
C6 C5 C7 106.5(3) . . ?
C6 C5 C8 109.4(3) . . ?
C8 C5 C7 109.5(3) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
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
C1 N1 1.474(4) . ?
C1 C2 1.531(5) . ?
C1 C3 1.542(5) . ?
C1 C4 1.530(5) . ?
N1 Pb1 2.215(3) . ?
N1 Si1 1.701(3) . ?
Pb1 Pb1 3.6310(10) 7_556 ?
Pb1 Si1 3.0116(11) . ?
Pb1 N2 2.343(3) . ?
Pb1 N2 2.540(3) 7_556 ?
Si1 N2 1.778(3) . ?
Si1 C9 1.887(4) . ?
Si1 C10 1.887(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
N2 Pb1 2.540(3) 7_556 ?
N2 C5 1.501(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.520(5) . ?
C5 C7 1.532(5) . ?
C5 C8 1.528(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
