#------------------------------------------------------------------------------
#$Date: 2022-05-21 01:03:45 +0300 (Sat, 21 May 2022) $
#$Revision: 275582 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/01/7130130.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_7130130
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                104.739(7)
_cell_angle_beta                 105.642(6)
_cell_angle_gamma                90.148(7)
_cell_formula_units_Z            2
_cell_length_a                   7.6866(15)
_cell_length_b                   11.591(3)
_cell_length_c                   12.678(3)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      27.70
_cell_measurement_theta_min      2.76
_cell_volume                     1048.8(4)
_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      100.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_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  0.0661
_diffrn_reflns_av_unetI/netI     0.0706
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_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            13799
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.831
_diffrn_reflns_theta_min         2.155
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.149
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1480 before and 0.0875 after correction.
The Ratio of minimum to maximum transmission is 0.3383.
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    2.116
_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         1.568
_refine_diff_density_min         -2.184
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0355
_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)+(0.0309P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0885
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4359
_reflns_number_total             4890
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc01522f2.cif
_cod_data_source_block           a
_cod_original_cell_volume        1048.9(4)
_cod_database_code               7130130
_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   0.461
_shelx_estimated_absorpt_t_min   0.341
_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), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B)
;
_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 0.62549(2) 0.30777(2) 0.22481(2) 0.01675(8) Uani 1 1 d . . . . .
Cl4 Cl 0.71979(18) 0.26610(13) 0.04206(11) 0.0236(3) Uani 1 1 d . . . . .
O1 O 0.6495(5) 0.0789(3) 0.2256(3) 0.0210(8) Uani 1 1 d . . . . .
O2 O 0.3377(5) 0.1434(3) 0.0999(3) 0.0218(8) Uani 1 1 d . . . . .
O3 O 0.2951(5) 0.3843(4) 0.1157(3) 0.0241(9) Uani 1 1 d . . . . .
O4 O 0.6041(5) 0.5403(3) 0.1983(3) 0.0247(9) Uani 1 1 d . . . . .
O5 O 0.9160(5) 0.4751(4) 0.3322(3) 0.0244(9) Uani 1 1 d . . . . .
O6 O 0.9538(5) 0.2340(3) 0.3080(3) 0.0217(8) Uani 1 1 d . . . . .
C1 C 0.5089(7) -0.0108(5) 0.1559(5) 0.0224(12) Uani 1 1 d . . . . .
H1A H 0.511351 -0.079185 0.189736 0.027 Uiso 1 1 calc R U . . .
H1B H 0.525903 -0.040493 0.079211 0.027 Uiso 1 1 calc R U . . .
C2 C 0.3327(7) 0.0445(5) 0.1485(5) 0.0233(12) Uani 1 1 d . . . . .
H2A H 0.231535 -0.014923 0.100165 0.028 Uiso 1 1 calc R U . . .
H2B H 0.314686 0.072793 0.225069 0.028 Uiso 1 1 calc R U . . .
C3 C 0.1626(7) 0.1864(5) 0.0660(5) 0.0238(12) Uani 1 1 d . . . . .
H3A H 0.111153 0.209000 0.131427 0.029 Uiso 1 1 calc R U . . .
H3B H 0.079625 0.123230 0.005463 0.029 Uiso 1 1 calc R U . . .
C4 C 0.1835(8) 0.2926(6) 0.0233(5) 0.0262(13) Uani 1 1 d . . . . .
H4A H 0.240632 0.270969 -0.039608 0.031 Uiso 1 1 calc R U . . .
H4B H 0.063339 0.321470 -0.005518 0.031 Uiso 1 1 calc R U . . .
C5 C 0.2978(8) 0.4953(5) 0.0870(5) 0.0272(13) Uani 1 1 d . . . . .
H5A H 0.174818 0.524275 0.072278 0.033 Uiso 1 1 calc R U . . .
H5B H 0.338232 0.484949 0.017534 0.033 Uiso 1 1 calc R U . . .
C6 C 0.4266(8) 0.5840(5) 0.1850(5) 0.0269(13) Uani 1 1 d . . . . .
H6A H 0.426951 0.663478 0.169443 0.032 Uiso 1 1 calc R U . . .
H6B H 0.389319 0.591962 0.255265 0.032 Uiso 1 1 calc R U . . .
C7 C 0.7405(9) 0.6286(5) 0.2751(5) 0.0292(14) Uani 1 1 d . . . . .
H7A H 0.717269 0.652505 0.350460 0.035 Uiso 1 1 calc R U . . .
H7B H 0.740270 0.700423 0.246344 0.035 Uiso 1 1 calc R U . . .
C8 C 0.9190(9) 0.5756(6) 0.2846(6) 0.0333(15) Uani 1 1 d . . . . .
H8A H 0.939964 0.548738 0.208674 0.040 Uiso 1 1 calc R U . . .
H8B H 1.017966 0.636013 0.334235 0.040 Uiso 1 1 calc R U . . .
C9 C 1.0911(8) 0.4302(5) 0.3576(6) 0.0294(14) Uani 1 1 d . . . . .
H9A H 1.179017 0.491882 0.416628 0.035 Uiso 1 1 calc R U . . .
H9B H 1.134054 0.408775 0.288642 0.035 Uiso 1 1 calc R U . . .
C10 C 1.0752(7) 0.3223(5) 0.3991(5) 0.0270(13) Uani 1 1 d . . . . .
H10A H 1.195537 0.291009 0.421500 0.032 Uiso 1 1 calc R U . . .
H10B H 1.027128 0.342926 0.466031 0.032 Uiso 1 1 calc R U . . .
C11 C 0.9567(7) 0.1197(5) 0.3317(5) 0.0229(12) Uani 1 1 d . . . . .
H11A H 0.922626 0.125698 0.402793 0.027 Uiso 1 1 calc R U . . .
H11B H 1.079780 0.091139 0.341254 0.027 Uiso 1 1 calc R U . . .
C12 C 0.8245(7) 0.0346(5) 0.2344(5) 0.0254(13) Uani 1 1 d . . . . .
H12A H 0.858179 0.028721 0.163212 0.031 Uiso 1 1 calc R U . . .
H12B H 0.824229 -0.046049 0.247481 0.031 Uiso 1 1 calc R U . . .
Mn1 Mn 0.63012(11) 0.13029(8) 0.55954(7) 0.02077(19) Uani 1 1 d . . . . .
Cl1 Cl 0.67048(18) -0.06292(12) 0.44002(12) 0.0237(3) Uani 1 1 d . . . . .
Cl2 Cl 0.83855(18) 0.16944(13) 0.73600(12) 0.0262(3) Uani 1 1 d . . . . .
Cl3 Cl 0.5964(2) 0.28978(13) 0.47672(12) 0.0279(3) 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'
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 O1 90.44(9) . . ?
Cl4 Pb1 O2 85.11(9) . . ?
Cl4 Pb1 O3 90.25(9) . . ?
Cl4 Pb1 O4 83.04(9) . . ?
Cl4 Pb1 O5 90.28(9) . . ?
Cl4 Pb1 O6 83.28(9) . . ?
O1 Pb1 O2 60.26(11) . . ?
O1 Pb1 O3 119.77(11) . . ?
O1 Pb1 O4 173.35(11) . . ?
O1 Pb1 O5 121.78(11) . . ?
O1 Pb1 O6 61.52(11) . . ?
O2 Pb1 O3 59.82(11) . . ?
O2 Pb1 O4 117.60(11) . . ?
O2 Pb1 O5 175.03(10) . . ?
O4 Pb1 O3 59.22(11) . . ?
O5 Pb1 O3 118.44(12) . . ?
O5 Pb1 O4 59.79(11) . . ?
O6 Pb1 O2 120.31(11) . . ?
O6 Pb1 O3 173.45(11) . . ?
O6 Pb1 O4 118.65(12) . . ?
O6 Pb1 O5 60.80(12) . . ?
C1 O1 Pb1 121.7(3) . . ?
C12 O1 Pb1 116.4(3) . . ?
C12 O1 C1 111.5(4) . . ?
C2 O2 Pb1 111.9(3) . . ?
C3 O2 Pb1 118.3(3) . . ?
C3 O2 C2 112.1(4) . . ?
C4 O3 Pb1 113.7(3) . . ?
C5 O3 Pb1 118.2(3) . . ?
C5 O3 C4 111.5(4) . . ?
C6 O4 Pb1 114.7(3) . . ?
C7 O4 Pb1 117.0(3) . . ?
C7 O4 C6 111.4(4) . . ?
C8 O5 Pb1 115.8(3) . . ?
C9 O5 Pb1 116.6(3) . . ?
C9 O5 C8 110.8(5) . . ?
C10 O6 Pb1 114.7(3) . . ?
C11 O6 Pb1 116.6(3) . . ?
C11 O6 C10 111.6(4) . . ?
O1 C1 H1A 110.2 . . ?
O1 C1 H1B 110.2 . . ?
O1 C1 C2 107.7(5) . . ?
H1A C1 H1B 108.5 . . ?
C2 C1 H1A 110.2 . . ?
C2 C1 H1B 110.2 . . ?
O2 C2 C1 107.6(4) . . ?
O2 C2 H2A 110.2 . . ?
O2 C2 H2B 110.2 . . ?
C1 C2 H2A 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
O2 C3 H3A 110.1 . . ?
O2 C3 H3B 110.1 . . ?
O2 C3 C4 108.1(4) . . ?
H3A C3 H3B 108.4 . . ?
C4 C3 H3A 110.1 . . ?
C4 C3 H3B 110.1 . . ?
O3 C4 C3 108.1(4) . . ?
O3 C4 H4A 110.1 . . ?
O3 C4 H4B 110.1 . . ?
C3 C4 H4A 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
O3 C5 H5A 110.1 . . ?
O3 C5 H5B 110.1 . . ?
O3 C5 C6 108.1(5) . . ?
H5A C5 H5B 108.4 . . ?
C6 C5 H5A 110.1 . . ?
C6 C5 H5B 110.1 . . ?
O4 C6 C5 107.5(5) . . ?
O4 C6 H6A 110.2 . . ?
O4 C6 H6B 110.2 . . ?
C5 C6 H6A 110.2 . . ?
C5 C6 H6B 110.2 . . ?
H6A C6 H6B 108.5 . . ?
O4 C7 H7A 110.1 . . ?
O4 C7 H7B 110.1 . . ?
O4 C7 C8 107.9(5) . . ?
H7A C7 H7B 108.4 . . ?
C8 C7 H7A 110.1 . . ?
C8 C7 H7B 110.1 . . ?
O5 C8 C7 108.1(5) . . ?
O5 C8 H8A 110.1 . . ?
O5 C8 H8B 110.1 . . ?
C7 C8 H8A 110.1 . . ?
C7 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
O5 C9 H9A 110.1 . . ?
O5 C9 H9B 110.1 . . ?
O5 C9 C10 107.8(5) . . ?
H9A C9 H9B 108.5 . . ?
C10 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
O6 C10 C9 107.6(5) . . ?
O6 C10 H10A 110.2 . . ?
O6 C10 H10B 110.2 . . ?
C9 C10 H10A 110.2 . . ?
C9 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
O6 C11 H11A 110.1 . . ?
O6 C11 H11B 110.1 . . ?
O6 C11 C12 108.0(4) . . ?
H11A C11 H11B 108.4 . . ?
C12 C11 H11A 110.1 . . ?
C12 C11 H11B 110.1 . . ?
O1 C12 C11 107.8(5) . . ?
O1 C12 H12A 110.2 . . ?
O1 C12 H12B 110.2 . . ?
C11 C12 H12A 110.2 . . ?
C11 C12 H12B 110.2 . . ?
H12A C12 H12B 108.5 . . ?
Cl1 Mn1 Cl1 92.23(5) . 2_656 ?
Cl2 Mn1 Cl1 110.65(6) . . ?
Cl2 Mn1 Cl1 113.04(6) . 2_656 ?
Cl2 Mn1 Cl3 114.78(6) . . ?
Cl3 Mn1 Cl1 107.45(6) . 2_656 ?
Cl3 Mn1 Cl1 116.53(6) . . ?
Mn1 Cl1 Mn1 87.77(5) . 2_656 ?
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 2.5426(14) . ?
Pb1 O1 2.662(4) . ?
Pb1 O2 2.754(4) . ?
Pb1 O3 2.809(4) . ?
Pb1 O4 2.800(4) . ?
Pb1 O5 2.756(4) . ?
Pb1 O6 2.692(4) . ?
O1 C1 1.429(6) . ?
O1 C12 1.427(6) . ?
O2 C2 1.438(6) . ?
O2 C3 1.430(6) . ?
O3 C4 1.434(7) . ?
O3 C5 1.425(7) . ?
O4 C6 1.439(7) . ?
O4 C7 1.425(7) . ?
O5 C8 1.445(7) . ?
O5 C9 1.428(7) . ?
O6 C10 1.437(7) . ?
O6 C11 1.430(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.490(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.489(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.504(9) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.492(9) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.492(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.493(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
Mn1 Cl1 2.4368(17) . ?
Mn1 Cl1 2.4390(16) 2_656 ?
Mn1 Cl2 2.3075(17) . ?
Mn1 Cl3 2.3305(16) . ?
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 O1 C1 C2 -34.5(5) . . . . ?
Pb1 O1 C12 C11 49.9(5) . . . . ?
Pb1 O2 C2 C1 -57.3(5) . . . . ?
Pb1 O2 C3 C4 44.3(5) . . . . ?
Pb1 O3 C4 C3 52.7(5) . . . . ?
Pb1 O3 C5 C6 -41.8(5) . . . . ?
Pb1 O4 C6 C5 -55.0(5) . . . . ?
Pb1 O4 C7 C8 44.7(6) . . . . ?
Pb1 O5 C8 C7 52.1(6) . . . . ?
Pb1 O5 C9 C10 -41.1(6) . . . . ?
Pb1 O6 C10 C9 -55.8(5) . . . . ?
Pb1 O6 C11 C12 44.3(5) . . . . ?
O1 C1 C2 O2 59.3(6) . . . . ?
O2 C3 C4 O3 -63.4(6) . . . . ?
O3 C5 C6 O4 62.8(6) . . . . ?
O4 C7 C8 O5 -62.7(6) . . . . ?
O5 C9 C10 O6 62.8(6) . . . . ?
O6 C11 C12 O1 -60.6(6) . . . . ?
C1 O1 C12 C11 -164.4(4) . . . . ?
C2 O2 C3 C4 176.7(4) . . . . ?
C3 O2 C2 C1 167.2(5) . . . . ?
C4 O3 C5 C6 -176.4(4) . . . . ?
C5 O3 C4 C3 -170.6(4) . . . . ?
C6 O4 C7 C8 179.5(5) . . . . ?
C7 O4 C6 C5 169.2(5) . . . . ?
C8 O5 C9 C10 -176.4(5) . . . . ?
C9 O5 C8 C7 -172.3(5) . . . . ?
C10 O6 C11 C12 178.8(4) . . . . ?
C11 O6 C10 C9 168.8(4) . . . . ?
C12 O1 C1 C2 -178.1(4) . . . . ?
