#------------------------------------------------------------------------------
#$Date: 2022-05-21 01:03:45 +0300 (Sat, 21 May 2022) $
#$Revision: 275582 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/01/7130131.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_7130131
loop_
_publ_author_name
'Zhang, Liming'
'Luo, Zhishan'
'Wei, Yi'
'Wang, Wei'
'Liu, Yulian'
'Li, Chen'
'He, Xin'
'Quan, Zewei'
_publ_section_title
;
 Zero-Dimensional Hybrid Binuclear Manganese Chloride with Thermally
 Stable Yellow Emission
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01522F
_journal_year                    2022
_chemical_formula_moiety         'C12 H24 Cl O6 Pb, Cl3 Mn'
_chemical_formula_sum            'C12 H24 Cl4 Mn O6 Pb'
_chemical_formula_weight         668.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-02-20 deposited with the CCDC.	2022-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                103.837(14)
_cell_angle_beta                 107.563(13)
_cell_angle_gamma                90.337(14)
_cell_formula_units_Z            2
_cell_length_a                   7.883(3)
_cell_length_b                   11.619(5)
_cell_length_c                   13.058(5)
_cell_measurement_reflns_used    8651
_cell_measurement_temperature    400.0
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.72
_cell_volume                     1103.2(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      400.0
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.961
_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  0.0698
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10400
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.278
_diffrn_reflns_theta_min         2.143
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.698
_exptl_absorpt_correction_T_max  0.0908
_exptl_absorpt_correction_T_min  0.0336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1504 before and 0.1040 after correction.
The Ratio of minimum to maximum transmission is 0.3700.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_description       block
_exptl_crystal_F_000             638
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.0
_refine_diff_density_max         2.493
_refine_diff_density_min         -3.511
_refine_diff_density_rms         0.317
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0763
_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)+(0.1407P)²+5.9054P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2007
_refine_ls_wR_factor_ref         0.2169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3307
_reflns_number_total             3860
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc01522f2.cif
_cod_data_source_block           pmc186_0m
_cod_database_code               7130131
_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.
;
_shelx_estimated_absorpt_t_max   1.000
_shelx_estimated_absorpt_t_min   0.355
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C8(H8A,H8B), C7(H7A,H7B), C12(H12A,H12B), C11(H11A,H11B), C4(H4A,
 H4B), C10(H10A,H10B), C9(H9A,H9B), C1(H1A,H1B), C6(H6A,H6B), C3(H3A,H3B),
 C5(H5A,H5B)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_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 0.37329(6) 0.69253(4) 0.77509(4) 0.0496(3) Uani 1 1 d . . . . .
Mn1 Mn 0.3717(3) 0.8678(2) 0.4430(2) 0.0609(6) Uani 1 1 d . . . . .
Cl1 Cl 0.3344(5) 1.0610(4) 0.5566(4) 0.0677(10) Uani 1 1 d . . . . .
Cl4 Cl 0.2888(6) 0.7295(4) 0.9524(4) 0.0749(11) Uani 1 1 d . . . . .
Cl2 Cl 0.1640(7) 0.8276(4) 0.2686(5) 0.0808(12) Uani 1 1 d . . . . .
Cl3 Cl 0.4090(8) 0.7124(4) 0.5292(4) 0.0826(13) Uani 1 1 d . . . . .
O5 O 0.7068(18) 0.6212(13) 0.8824(12) 0.080(4) Uani 1 1 d . . . . .
O6 O 0.6603(17) 0.8577(11) 0.8949(13) 0.079(4) Uani 1 1 d . . . . .
O3 O 0.089(2) 0.5253(14) 0.6703(13) 0.090(4) Uani 1 1 d . . . . .
O1 O 0.343(2) 0.9218(11) 0.7735(14) 0.083(4) Uani 1 1 d . . . . .
O4 O 0.406(3) 0.4605(10) 0.7988(13) 0.093(5) Uani 1 1 d . . . . .
O2 O 0.0490(18) 0.7665(14) 0.6922(12) 0.083(4) Uani 1 1 d . . . . .
C2 C 0.048(3) 0.881(2) 0.667(2) 0.087(6) Uani 1 1 d . . . . .
H2A H 0.082834 0.875566 0.601346 0.105 Uiso 1 1 calc R U . . .
H2B H -0.070603 0.908733 0.654507 0.105 Uiso 1 1 calc R U . . .
C8 C 0.705(4) 0.508(2) 0.906(3) 0.107(9) Uani 1 1 d . . . . .
H8A H 0.671645 0.514296 0.972966 0.128 Uiso 1 1 calc R U . . .
H8B H 0.824012 0.479813 0.919510 0.128 Uiso 1 1 calc R U . . .
C7 C 0.580(4) 0.423(2) 0.814(2) 0.111(9) Uani 1 1 d . . . . .
H7A H 0.612563 0.417050 0.747334 0.134 Uiso 1 1 calc R U . . .
H7B H 0.583822 0.345059 0.829344 0.134 Uiso 1 1 calc R U . . .
C12 C 0.487(3) 1.0110(18) 0.8447(19) 0.085(6) Uani 1 1 d . . . . .
H12A H 0.475158 1.036379 0.918332 0.102 Uiso 1 1 calc R U . . .
H12B H 0.482868 1.079993 0.814546 0.102 Uiso 1 1 calc R U . . .
C11 C 0.659(3) 0.9581(19) 0.851(2) 0.091(7) Uani 1 1 d . . . . .
H11A H 0.672318 0.934251 0.777465 0.109 Uiso 1 1 calc R U . . .
H11B H 0.757425 1.015865 0.898244 0.109 Uiso 1 1 calc R U . . .
C4 C -0.089(3) 0.572(2) 0.638(3) 0.112(10) Uani 1 1 d . . . . .
H4A H -0.170849 0.513208 0.577434 0.135 Uiso 1 1 calc R U . . .
H4B H -0.135131 0.587859 0.700440 0.135 Uiso 1 1 calc R U . . .
C10 C 0.833(3) 0.816(2) 0.930(2) 0.093(7) Uani 1 1 d . . . . .
H10A H 0.913036 0.877131 0.989057 0.112 Uiso 1 1 calc R U . . .
H10B H 0.881296 0.796838 0.868378 0.112 Uiso 1 1 calc R U . . .
C9 C 0.817(3) 0.709(2) 0.970(2) 0.100(7) Uani 1 1 d . . . . .
H9A H 0.934487 0.680665 0.995945 0.120 Uiso 1 1 calc R U . . .
H9B H 0.767832 0.727294 1.030599 0.120 Uiso 1 1 calc R U . . .
C1 C 0.172(3) 0.962(2) 0.760(2) 0.099(7) Uani 1 1 d . . . . .
H1A H 0.170331 1.041034 0.748079 0.118 Uiso 1 1 calc R U . . .
H1B H 0.138914 0.965369 0.826814 0.118 Uiso 1 1 calc R U . . .
C6 C 0.262(4) 0.3730(18) 0.722(2) 0.110(9) Uani 1 1 d . . . . .
H6A H 0.260625 0.302148 0.748336 0.131 Uiso 1 1 calc R U . . .
H6B H 0.278337 0.350593 0.648939 0.131 Uiso 1 1 calc R U . . .
C3 C -0.073(3) 0.681(2) 0.604(2) 0.101(8) Uani 1 1 d . . . . .
H3A H -0.032412 0.664190 0.539457 0.121 Uiso 1 1 calc R U . . .
H3B H -0.189499 0.711952 0.584049 0.121 Uiso 1 1 calc R U . . .
C5 C 0.092(5) 0.429(3) 0.714(2) 0.130(12) Uani 1 1 d . . . . .
H5A H -0.007461 0.371354 0.667719 0.156 Uiso 1 1 calc R U . . .
H5B H 0.078774 0.454072 0.787619 0.156 Uiso 1 1 calc R 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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
Cl4 Pb1 O5 90.9(3) . . ?
Cl4 Pb1 O6 86.3(3) . . ?
Cl4 Pb1 O3 90.0(3) . . ?
Cl4 Pb1 O1 90.4(3) . . ?
Cl4 Pb1 O4 84.2(3) . . ?
Cl4 Pb1 O2 83.5(3) . . ?
O6 Pb1 O5 59.0(4) . . ?
O6 Pb1 O4 117.3(5) . . ?
O3 Pb1 O5 119.3(5) . . ?
O3 Pb1 O6 175.9(4) . . ?
O3 Pb1 O4 60.4(5) . . ?
O1 Pb1 O5 119.2(5) . . ?
O1 Pb1 O6 60.4(5) . . ?
O1 Pb1 O3 121.5(5) . . ?
O1 Pb1 O4 174.3(4) . . ?
O1 Pb1 O2 60.5(5) . . ?
O4 Pb1 O5 59.4(5) . . ?
O2 Pb1 O5 174.3(4) . . ?
O2 Pb1 O6 119.8(4) . . ?
O2 Pb1 O3 61.5(5) . . ?
O2 Pb1 O4 120.3(5) . . ?
Cl1 Mn1 Cl1 91.69(15) . 2_676 ?
Cl2 Mn1 Cl1 112.1(2) . 2_676 ?
Cl2 Mn1 Cl1 110.79(19) . . ?
Cl2 Mn1 Cl3 115.7(2) . . ?
Cl3 Mn1 Cl1 115.7(2) . . ?
Cl3 Mn1 Cl1 108.3(2) . 2_676 ?
Mn1 Cl1 Mn1 88.31(15) . 2_676 ?
C8 O5 Pb1 116.3(13) . . ?
C9 O5 Pb1 115.0(13) . . ?
C9 O5 C8 113(2) . . ?
C11 O6 Pb1 113.0(13) . . ?
C11 O6 C10 113.7(17) . . ?
C10 O6 Pb1 118.3(12) . . ?
C4 O3 Pb1 115.9(12) . . ?
C5 O3 Pb1 115.6(16) . . ?
C5 O3 C4 114(2) . . ?
C12 O1 Pb1 119.9(12) . . ?
C1 O1 Pb1 116.4(14) . . ?
C1 O1 C12 113.9(17) . . ?
C7 O4 Pb1 114.5(14) . . ?
C7 O4 C6 115.3(19) . . ?
C6 O4 Pb1 114.9(14) . . ?
C2 O2 Pb1 115.8(12) . . ?
C3 O2 Pb1 115.1(13) . . ?
C3 O2 C2 111.4(19) . . ?
O2 C2 H2A 110.2 . . ?
O2 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
C1 C2 O2 107.8(19) . . ?
C1 C2 H2A 110.2 . . ?
C1 C2 H2B 110.2 . . ?
O5 C8 H8A 109.7 . . ?
O5 C8 H8B 109.7 . . ?
O5 C8 C7 110(2) . . ?
H8A C8 H8B 108.2 . . ?
C7 C8 H8A 109.7 . . ?
C7 C8 H8B 109.7 . . ?
O4 C7 C8 109.5(19) . . ?
O4 C7 H7A 109.8 . . ?
O4 C7 H7B 109.8 . . ?
C8 C7 H7A 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
O1 C12 H12A 110.0 . . ?
O1 C12 H12B 110.0 . . ?
O1 C12 C11 108.4(17) . . ?
H12A C12 H12B 108.4 . . ?
C11 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
O6 C11 C12 108.4(16) . . ?
O6 C11 H11A 110.0 . . ?
O6 C11 H11B 110.0 . . ?
C12 C11 H11A 110.0 . . ?
C12 C11 H11B 110.0 . . ?
H11A C11 H11B 108.4 . . ?
O3 C4 H4A 109.7 . . ?
O3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C3 C4 O3 109.8(17) . . ?
C3 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
O6 C10 H10A 109.9 . . ?
O6 C10 H10B 109.9 . . ?
O6 C10 C9 109.1(17) . . ?
H10A C10 H10B 108.3 . . ?
C9 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
O5 C9 C10 109(2) . . ?
O5 C9 H9A 110.0 . . ?
O5 C9 H9B 110.0 . . ?
C10 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
H9A C9 H9B 108.3 . . ?
O1 C1 C2 108(2) . . ?
O1 C1 H1A 110.0 . . ?
O1 C1 H1B 110.0 . . ?
C2 C1 H1A 110.0 . . ?
C2 C1 H1B 110.0 . . ?
H1A C1 H1B 108.4 . . ?
O4 C6 H6A 110.2 . . ?
O4 C6 H6B 110.2 . . ?
O4 C6 C5 107.5(18) . . ?
H6A C6 H6B 108.5 . . ?
C5 C6 H6A 110.2 . . ?
C5 C6 H6B 110.2 . . ?
O2 C3 C4 110(2) . . ?
O2 C3 H3A 109.7 . . ?
O2 C3 H3B 109.7 . . ?
C4 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
O3 C5 C6 110(2) . . ?
O3 C5 H5A 109.6 . . ?
O3 C5 H5B 109.6 . . ?
C6 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
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 Cl4 2.540(4) . ?
Pb1 O5 2.814(13) . ?
Pb1 O6 2.762(13) . ?
Pb1 O3 2.738(13) . ?
Pb1 O1 2.681(12) . ?
Pb1 O4 2.791(11) . ?
Pb1 O2 2.692(14) . ?
Mn1 Cl1 2.454(5) 2_676 ?
Mn1 Cl1 2.451(5) . ?
Mn1 Cl2 2.306(6) . ?
Mn1 Cl3 2.322(5) . ?
O5 C8 1.43(3) . ?
O5 C9 1.39(3) . ?
O6 C11 1.42(3) . ?
O6 C10 1.43(3) . ?
O3 C4 1.48(3) . ?
O3 C5 1.37(3) . ?
O1 C12 1.45(3) . ?
O1 C1 1.41(3) . ?
O4 C7 1.41(3) . ?
O4 C6 1.47(3) . ?
O2 C2 1.44(3) . ?
O2 C3 1.42(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.43(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.45(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C11 1.48(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.45(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.48(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.48(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb1 O5 C8 C7 40(3) . . . . ?
Pb1 O5 C9 C10 -52(2) . . . . ?
Pb1 O6 C11 C12 55.9(18) . . . . ?
Pb1 O6 C10 C9 -42(2) . . . . ?
Pb1 O3 C4 C3 36(3) . . . . ?
Pb1 O3 C5 C6 -54(2) . . . . ?
Pb1 O1 C12 C11 36(2) . . . . ?
Pb1 O1 C1 C2 -50(2) . . . . ?
Pb1 O4 C7 C8 54(2) . . . . ?
Pb1 O4 C6 C5 -42(3) . . . . ?
Pb1 O2 C2 C1 -47(2) . . . . ?
Pb1 O2 C3 C4 54(2) . . . . ?
O5 C8 C7 O4 -62(3) . . . . ?
O6 C10 C9 O5 61(3) . . . . ?
O3 C4 C3 O2 -59(3) . . . . ?
O1 C12 C11 O6 -59(2) . . . . ?
O4 C6 C5 O3 63(3) . . . . ?
O2 C2 C1 O1 62(2) . . . . ?
C2 O2 C3 C4 -171.6(18) . . . . ?
C8 O5 C9 C10 170.5(19) . . . . ?
C7 O4 C6 C5 -179(2) . . . . ?
C12 O1 C1 C2 164.2(19) . . . . ?
C11 O6 C10 C9 -177.6(19) . . . . ?
C4 O3 C5 C6 168(2) . . . . ?
C10 O6 C11 C12 -165.7(18) . . . . ?
C9 O5 C8 C7 177(2) . . . . ?
C1 O1 C12 C11 -179.7(19) . . . . ?
C6 O4 C7 C8 -170(2) . . . . ?
C3 O2 C2 C1 179.1(19) . . . . ?
C5 O3 C4 C3 174(2) . . . . ?
