#------------------------------------------------------------------------------
#$Date: 2022-05-21 01:03:45 +0300 (Sat, 21 May 2022) $
#$Revision: 275582 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/01/7130132.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_7130132
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                104.638(2)
_cell_angle_beta                 105.858(2)
_cell_angle_gamma                90.193(2)
_cell_formula_units_Z            2
_cell_length_a                   7.7138(5)
_cell_length_b                   11.6050(8)
_cell_length_c                   12.7334(8)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    199.99
_cell_measurement_theta_max      27.69
_cell_measurement_theta_min      2.75
_cell_volume                     1057.69(12)
_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      199.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_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  0.0607
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14631
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.794
_diffrn_reflns_theta_min         2.151
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.073
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1498 before and 0.0861 after correction.
The Ratio of minimum to maximum transmission is 0.3509.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.098
_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          0.1
_refine_diff_density_max         1.098
_refine_diff_density_min         -2.079
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0327
_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)+(0.0230P)²+0.6791P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4576
_reflns_number_total             4933
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc01522f2.cif
_cod_data_source_block           pmc186_200_0m
_cod_database_code               7130132
_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   0.464
_shelx_estimated_absorpt_t_min   0.343
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B), C3(H3A,H3B), C5(H5A,H5B), C12(H12A,H12B), C8(H8A,
 H8B), C7(H7A,H7B), C2(H2A,H2B), C11(H11A,H11B), C10(H10A,H10B), C6(H6A,H6B),
 C9(H9A,H9B)
;
_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 0.62568(2) 0.30765(2) 0.22475(2) 0.02121(7) Uani 1 1 d . . . . .
Mn1 Mn 0.62992(10) 0.13072(6) 0.55921(6) 0.02699(16) Uani 1 1 d . . . . .
Cl1 Cl 0.33036(16) 0.06248(10) 0.55938(10) 0.0298(2) Uani 1 1 d . . . . .
Cl4 Cl 0.71883(16) 0.26650(11) 0.04286(10) 0.0306(3) Uani 1 1 d . . . . .
Cl2 Cl 0.83837(17) 0.16991(11) 0.73531(11) 0.0342(3) Uani 1 1 d . . . . .
Cl3 Cl 0.59551(19) 0.28947(11) 0.47584(11) 0.0365(3) Uani 1 1 d . . . . .
O2 O 0.6499(4) 0.0793(3) 0.2256(3) 0.0277(7) Uani 1 1 d . . . . .
O4 O 0.2945(5) 0.3830(3) 0.1161(3) 0.0311(8) Uani 1 1 d . . . . .
O1 O 0.9533(4) 0.2345(3) 0.3075(3) 0.0272(7) Uani 1 1 d . . . . .
O5 O 0.6026(5) 0.5394(3) 0.1983(3) 0.0330(8) Uani 1 1 d . . . . .
O3 O 0.3384(4) 0.1430(3) 0.1005(3) 0.0291(7) Uani 1 1 d . . . . .
O6 O 0.9156(5) 0.4751(3) 0.3319(3) 0.0325(8) Uani 1 1 d . . . . .
C1 C 0.9560(7) 0.1207(5) 0.3321(4) 0.0322(11) Uani 1 1 d . . . . .
H1A H 0.921620 0.127116 0.402738 0.039 Uiso 1 1 calc R U . . .
H1B H 1.078788 0.092195 0.342339 0.039 Uiso 1 1 calc R U . . .
C4 C 0.3340(7) 0.0441(5) 0.1485(5) 0.0324(11) Uani 1 1 d . . . . .
H4A H 0.233146 -0.015313 0.100209 0.039 Uiso 1 1 calc R U . . .
H4B H 0.316527 0.071946 0.224821 0.039 Uiso 1 1 calc R U . . .
C3 C 0.5098(7) -0.0102(4) 0.1556(4) 0.0302(11) Uani 1 1 d . . . . .
H3A H 0.512935 -0.079054 0.188677 0.036 Uiso 1 1 calc R U . . .
H3B H 0.526459 -0.038875 0.079164 0.036 Uiso 1 1 calc R U . . .
C5 C 0.1638(7) 0.1862(5) 0.0677(5) 0.0335(11) Uani 1 1 d . . . . .
H5A H 0.113850 0.208666 0.133233 0.040 Uiso 1 1 calc R U . . .
H5B H 0.080026 0.123433 0.007461 0.040 Uiso 1 1 calc R U . . .
C12 C 1.0743(7) 0.3220(5) 0.3974(5) 0.0383(13) Uani 1 1 d . . . . .
H12A H 1.194459 0.290768 0.419343 0.046 Uiso 1 1 calc R U . . .
H12B H 1.027436 0.342280 0.464353 0.046 Uiso 1 1 calc R U . . .
C8 C 0.4273(8) 0.5826(5) 0.1851(5) 0.0383(13) Uani 1 1 d . . . . .
H8A H 0.427645 0.662000 0.169584 0.046 Uiso 1 1 calc R U . . .
H8B H 0.390761 0.590563 0.255187 0.046 Uiso 1 1 calc R U . . .
C7 C 0.2969(7) 0.4939(5) 0.0871(5) 0.0372(13) Uani 1 1 d . . . . .
H7A H 0.174361 0.523008 0.072638 0.045 Uiso 1 1 calc R U . . .
H7B H 0.336315 0.483401 0.017696 0.045 Uiso 1 1 calc R U . . .
C2 C 0.8250(7) 0.0359(4) 0.2355(5) 0.0313(11) Uani 1 1 d . . . . .
H2A H 0.858858 0.030088 0.164891 0.038 Uiso 1 1 calc R U . . .
H2B H 0.825034 -0.044505 0.248859 0.038 Uiso 1 1 calc R U . . .
C11 C 1.0893(7) 0.4300(5) 0.3563(5) 0.0397(13) Uani 1 1 d . . . . .
H11A H 1.177868 0.491245 0.415039 0.048 Uiso 1 1 calc R U . . .
H11B H 1.130942 0.408792 0.287348 0.048 Uiso 1 1 calc R U . . .
C10 C 0.9161(8) 0.5745(5) 0.2849(5) 0.0433(14) Uani 1 1 d . . . . .
H10A H 0.935705 0.547991 0.209050 0.052 Uiso 1 1 calc R U . . .
H10B H 1.015028 0.635013 0.334032 0.052 Uiso 1 1 calc R U . . .
C6 C 0.1845(7) 0.2926(5) 0.0252(5) 0.0360(12) Uani 1 1 d . . . . .
H6A H 0.241339 0.271215 -0.037305 0.043 Uiso 1 1 calc R U . . .
H6B H 0.064566 0.321306 -0.003686 0.043 Uiso 1 1 calc R U . . .
C9 C 0.7390(9) 0.6268(5) 0.2761(5) 0.0443(14) Uani 1 1 d . . . . .
H9A H 0.716015 0.648949 0.351212 0.053 Uiso 1 1 calc R U . . .
H9B H 0.738775 0.699580 0.249013 0.053 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 O2 90.44(8) . . ?
Cl4 Pb1 O4 90.45(8) . . ?
Cl4 Pb1 O1 83.19(8) . . ?
Cl4 Pb1 O5 83.13(8) . . ?
Cl4 Pb1 O3 85.21(8) . . ?
Cl4 Pb1 O6 90.26(8) . . ?
O2 Pb1 O4 119.53(10) . . ?
O2 Pb1 O1 61.60(10) . . ?
O2 Pb1 O5 173.41(10) . . ?
O2 Pb1 O3 60.17(10) . . ?
O2 Pb1 O6 121.81(10) . . ?
O1 Pb1 O4 173.59(9) . . ?
O1 Pb1 O5 118.76(10) . . ?
O1 Pb1 O3 120.30(10) . . ?
O1 Pb1 O6 60.76(10) . . ?
O5 Pb1 O4 59.30(10) . . ?
O3 Pb1 O4 59.68(10) . . ?
O3 Pb1 O5 117.53(10) . . ?
O3 Pb1 O6 175.11(9) . . ?
O6 Pb1 O4 118.65(10) . . ?
O6 Pb1 O5 59.94(10) . . ?
Cl1 Mn1 Cl1 91.99(5) 2_656 . ?
Cl2 Mn1 Cl1 110.61(5) . 2_656 ?
Cl2 Mn1 Cl1 112.98(5) . . ?
Cl2 Mn1 Cl3 114.98(5) . . ?
Cl3 Mn1 Cl1 116.46(5) . 2_656 ?
Cl3 Mn1 Cl1 107.58(5) . . ?
Mn1 Cl1 Mn1 88.01(5) 2_656 . ?
C3 O2 Pb1 121.5(3) . . ?
C2 O2 Pb1 116.2(3) . . ?
C2 O2 C3 111.9(4) . . ?
C7 O4 Pb1 118.0(3) . . ?
C6 O4 Pb1 113.8(3) . . ?
C6 O4 C7 111.4(4) . . ?
C1 O1 Pb1 116.4(3) . . ?
C12 O1 Pb1 114.9(3) . . ?
C12 O1 C1 111.3(4) . . ?
C8 O5 Pb1 115.0(3) . . ?
C8 O5 C9 111.5(4) . . ?
C9 O5 Pb1 116.1(3) . . ?
C4 O3 Pb1 112.0(3) . . ?
C5 O3 Pb1 118.0(3) . . ?
C5 O3 C4 112.0(4) . . ?
C11 O6 Pb1 116.3(3) . . ?
C11 O6 C10 111.4(4) . . ?
C10 O6 Pb1 115.3(3) . . ?
O1 C1 H1A 110.2 . . ?
O1 C1 H1B 110.2 . . ?
O1 C1 C2 107.8(4) . . ?
H1A C1 H1B 108.5 . . ?
C2 C1 H1A 110.2 . . ?
C2 C1 H1B 110.2 . . ?
O3 C4 H4A 110.2 . . ?
O3 C4 H4B 110.2 . . ?
O3 C4 C3 107.4(4) . . ?
H4A C4 H4B 108.5 . . ?
C3 C4 H4A 110.2 . . ?
C3 C4 H4B 110.2 . . ?
O2 C3 C4 107.8(4) . . ?
O2 C3 H3A 110.1 . . ?
O2 C3 H3B 110.1 . . ?
C4 C3 H3A 110.1 . . ?
C4 C3 H3B 110.1 . . ?
H3A C3 H3B 108.5 . . ?
O3 C5 H5A 110.1 . . ?
O3 C5 H5B 110.1 . . ?
O3 C5 C6 107.9(4) . . ?
H5A C5 H5B 108.4 . . ?
C6 C5 H5A 110.1 . . ?
C6 C5 H5B 110.1 . . ?
O1 C12 H12A 110.2 . . ?
O1 C12 H12B 110.2 . . ?
O1 C12 C11 107.7(4) . . ?
H12A C12 H12B 108.5 . . ?
C11 C12 H12A 110.2 . . ?
C11 C12 H12B 110.2 . . ?
O5 C8 H8A 110.2 . . ?
O5 C8 H8B 110.2 . . ?
O5 C8 C7 107.7(4) . . ?
H8A C8 H8B 108.5 . . ?
C7 C8 H8A 110.2 . . ?
C7 C8 H8B 110.2 . . ?
O4 C7 C8 107.9(4) . . ?
O4 C7 H7A 110.1 . . ?
O4 C7 H7B 110.1 . . ?
C8 C7 H7A 110.1 . . ?
C8 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
O2 C2 C1 108.1(4) . . ?
O2 C2 H2A 110.1 . . ?
O2 C2 H2B 110.1 . . ?
C1 C2 H2A 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
O6 C11 C12 108.0(4) . . ?
O6 C11 H11A 110.1 . . ?
O6 C11 H11B 110.1 . . ?
C12 C11 H11A 110.1 . . ?
C12 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
O6 C10 H10A 110.0 . . ?
O6 C10 H10B 110.0 . . ?
O6 C10 C9 108.4(5) . . ?
H10A C10 H10B 108.4 . . ?
C9 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
O4 C6 C5 108.2(4) . . ?
O4 C6 H6A 110.1 . . ?
O4 C6 H6B 110.1 . . ?
C5 C6 H6A 110.1 . . ?
C5 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
O5 C9 C10 107.9(5) . . ?
O5 C9 H9A 110.1 . . ?
O5 C9 H9B 110.1 . . ?
C10 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
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 2.5420(11) . ?
Pb1 O2 2.660(3) . ?
Pb1 O4 2.811(3) . ?
Pb1 O1 2.689(3) . ?
Pb1 O5 2.795(3) . ?
Pb1 O3 2.755(3) . ?
Pb1 O6 2.757(3) . ?
Mn1 Cl1 2.4387(14) 2_656 ?
Mn1 Cl1 2.4409(14) . ?
Mn1 Cl2 2.3086(15) . ?
Mn1 Cl3 2.3300(14) . ?
O2 C3 1.428(6) . ?
O2 C2 1.427(6) . ?
O4 C7 1.427(6) . ?
O4 C6 1.416(6) . ?
O1 C1 1.432(6) . ?
O1 C12 1.426(6) . ?
O5 C8 1.425(6) . ?
O5 C9 1.426(6) . ?
O3 C4 1.435(6) . ?
O3 C5 1.429(6) . ?
O6 C11 1.423(6) . ?
O6 C10 1.428(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.485(7) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C3 1.488(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.491(7) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.490(8) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C7 1.513(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C9 1.485(9) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
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 O2 C3 C4 -35.1(5) . . . . ?
Pb1 O2 C2 C1 49.6(4) . . . . ?
Pb1 O4 C7 C8 -41.8(5) . . . . ?
Pb1 O4 C6 C5 53.0(5) . . . . ?
Pb1 O1 C1 C2 44.9(5) . . . . ?
Pb1 O1 C12 C11 -55.5(5) . . . . ?
Pb1 O5 C8 C7 -54.9(5) . . . . ?
Pb1 O5 C9 C10 45.5(5) . . . . ?
Pb1 O3 C4 C3 -57.2(4) . . . . ?
Pb1 O3 C5 C6 44.5(5) . . . . ?
Pb1 O6 C11 C12 -41.3(5) . . . . ?
Pb1 O6 C10 C9 52.2(5) . . . . ?
O1 C1 C2 O2 -61.0(5) . . . . ?
O1 C12 C11 O6 63.0(5) . . . . ?
O5 C8 C7 O4 62.8(5) . . . . ?
O3 C4 C3 O2 59.6(5) . . . . ?
O3 C5 C6 O4 -64.0(5) . . . . ?
O6 C10 C9 O5 -63.9(6) . . . . ?
C1 O1 C12 C11 169.5(4) . . . . ?
C4 O3 C5 C6 176.8(4) . . . . ?
C3 O2 C2 C1 -164.7(4) . . . . ?
C5 O3 C4 C3 167.7(4) . . . . ?
C12 O1 C1 C2 179.1(4) . . . . ?
C8 O5 C9 C10 179.8(4) . . . . ?
C7 O4 C6 C5 -170.7(4) . . . . ?
C2 O2 C3 C4 -178.7(4) . . . . ?
C11 O6 C10 C9 -172.5(5) . . . . ?
C10 O6 C11 C12 -176.2(4) . . . . ?
C6 O4 C7 C8 -176.0(4) . . . . ?
C9 O5 C8 C7 170.2(4) . . . . ?
