#------------------------------------------------------------------------------
#$Date: 2022-05-21 01:03:45 +0300 (Sat, 21 May 2022) $
#$Revision: 275582 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/01/7130133.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_7130133
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             2022-02-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-20 deposited with the CCDC.	2022-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                104.333(2)
_cell_angle_beta                 106.573(2)
_cell_angle_gamma                90.283(2)
_cell_formula_units_Z            2
_cell_length_a                   7.7768(5)
_cell_length_b                   11.6166(7)
_cell_length_c                   12.8625(7)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    299.99
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.74
_cell_volume                     1075.48(11)
_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      299.99
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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  0.0578
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_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            15150
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.621
_diffrn_reflns_theta_min         2.147
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.923
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1378 before and 0.0856 after correction.
The Ratio of minimum to maximum transmission is 0.3562.
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    2.064
_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         -3.165
_refine_diff_density_rms         0.318
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0372
_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)+(0.0582P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4585
_reflns_number_total             4979
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc01522f2.cif
_cod_data_source_block           pmc186_300_0m
_cod_database_code               7130133
_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   0.469
_shelx_estimated_absorpt_t_min   0.348
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C10(H10A,H10B), C1(H1A,H1B), C6(H6A,H6B), C4(H4A,H4B),
 C11(H11A,H11B), C5(H5A,H5B), C2(H2A,H2B), C8(H8A,H8B), C9(H9A,H9B), C7(H7A,
 H7B), C3(H3A,H3B)
;
_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 0.37355(2) 0.69243(2) 0.77517(2) 0.03175(9) Uani 1 1 d . . . . .
Mn1 Mn 0.37095(13) 0.86860(8) 0.44183(8) 0.0402(2) Uani 1 1 d . . . . .
Cl4 Cl 0.2839(2) 0.73209(14) 0.95526(12) 0.0474(3) Uani 1 1 d . . . . .
Cl1 Cl 0.6678(2) 0.93826(13) 0.44185(13) 0.0445(3) Uani 1 1 d . . . . .
Cl2 Cl 0.1628(2) 0.82903(14) 0.26636(15) 0.0524(4) Uani 1 1 d . . . . .
Cl3 Cl 0.4064(3) 0.71135(15) 0.52617(14) 0.0550(4) Uani 1 1 d . . . . .
O6 O 0.6606(6) 0.8574(4) 0.8971(4) 0.0454(10) Uani 1 1 d . . . . .
O1 O 0.3471(6) 0.9206(4) 0.7740(4) 0.0445(10) Uani 1 1 d . . . . .
O4 O 0.4013(7) 0.4606(4) 0.7999(4) 0.0532(12) Uani 1 1 d . . . . .
O3 O 0.0862(7) 0.5251(4) 0.6691(4) 0.0532(12) Uani 1 1 d . . . . .
O5 O 0.7057(6) 0.6197(4) 0.8836(4) 0.0488(11) Uani 1 1 d . . . . .
O2 O 0.0475(6) 0.7648(4) 0.6914(4) 0.0464(10) Uani 1 1 d . . . . .
C12 C 0.4873(10) 1.0102(6) 0.8439(6) 0.0492(16) Uani 1 1 d . . . . .
H12A H 0.472714 1.037164 0.918353 0.059 Uiso 1 1 calc R U . . .
H12B H 0.482790 1.078076 0.812235 0.059 Uiso 1 1 calc R U . . .
C10 C 0.8339(9) 0.8162(7) 0.9322(7) 0.0548(17) Uani 1 1 d . . . . .
H10A H 0.913940 0.878282 0.991394 0.066 Uiso 1 1 calc R U . . .
H10B H 0.884078 0.795524 0.869667 0.066 Uiso 1 1 calc R U . . .
C1 C 0.1746(10) 0.9648(6) 0.7635(7) 0.0553(18) Uani 1 1 d . . . . .
H1A H 0.175085 1.042989 0.749368 0.066 Uiso 1 1 calc R U . . .
H1B H 0.142453 0.971522 0.832188 0.066 Uiso 1 1 calc R U . . .
C6 C 0.2601(14) 0.3739(6) 0.7231(7) 0.070(2) Uani 1 1 d . . . . .
H6A H 0.260244 0.303068 0.750198 0.083 Uiso 1 1 calc R U . . .
H6B H 0.280308 0.351184 0.649924 0.083 Uiso 1 1 calc R U . . .
C4 C -0.0887(9) 0.5698(7) 0.6406(8) 0.067(2) Uani 1 1 d . . . . .
H4A H -0.132544 0.588856 0.705844 0.080 Uiso 1 1 calc R U . . .
H4B H -0.173094 0.509732 0.581805 0.080 Uiso 1 1 calc R U . . .
C11 C 0.6620(10) 0.9572(6) 0.8507(7) 0.0545(17) Uani 1 1 d . . . . .
H11A H 0.677667 0.931526 0.776522 0.065 Uiso 1 1 calc R U . . .
H11B H 0.760353 1.015489 0.898195 0.065 Uiso 1 1 calc R U . . .
C5 C 0.0873(13) 0.4247(7) 0.7134(8) 0.072(2) Uani 1 1 d . . . . .
H5A H -0.008912 0.365644 0.664323 0.086 Uiso 1 1 calc R U . . .
H5B H 0.067942 0.448632 0.786741 0.086 Uiso 1 1 calc R U . . .
C2 C 0.0435(9) 0.8796(6) 0.6683(6) 0.0523(17) Uani 1 1 d . . . . .
H2A H -0.076446 0.906704 0.658734 0.063 Uiso 1 1 calc R U . . .
H2B H 0.074514 0.874437 0.599450 0.063 Uiso 1 1 calc R U . . .
C8 C 0.7030(11) 0.5071(7) 0.9109(7) 0.060(2) Uani 1 1 d . . . . .
H8A H 0.665276 0.516123 0.977925 0.073 Uiso 1 1 calc R U . . .
H8B H 0.822576 0.479007 0.925302 0.073 Uiso 1 1 calc R U . . .
C9 C 0.8161(10) 0.7096(8) 0.9740(7) 0.0587(19) Uani 1 1 d . . . . .
H9A H 0.933647 0.681910 1.001903 0.070 Uiso 1 1 calc R U . . .
H9B H 0.762192 0.729424 1.034909 0.070 Uiso 1 1 calc R U . . .
C7 C 0.5764(13) 0.4206(7) 0.8157(7) 0.068(2) Uani 1 1 d . . . . .
H7A H 0.612112 0.413460 0.748124 0.081 Uiso 1 1 calc R U . . .
H7B H 0.577513 0.342927 0.830977 0.081 Uiso 1 1 calc R U . . .
C3 C -0.0739(10) 0.6780(8) 0.6017(7) 0.064(2) Uani 1 1 d . . . . .
H3A H -0.029195 0.659247 0.536794 0.077 Uiso 1 1 calc R U . . .
H3B H -0.191043 0.708559 0.580333 0.077 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 O6 85.74(11) . . ?
Cl4 Pb1 O1 90.38(11) . . ?
Cl4 Pb1 O4 83.80(11) . . ?
Cl4 Pb1 O3 90.21(11) . . ?
Cl4 Pb1 O5 90.58(10) . . ?
Cl4 Pb1 O2 83.52(11) . . ?
O6 Pb1 O4 117.56(14) . . ?
O6 Pb1 O5 59.35(14) . . ?
O1 Pb1 O6 60.16(14) . . ?
O1 Pb1 O4 173.96(13) . . ?
O1 Pb1 O3 121.74(15) . . ?
O1 Pb1 O5 119.24(14) . . ?
O1 Pb1 O2 61.29(14) . . ?
O4 Pb1 O5 59.42(15) . . ?
O3 Pb1 O6 175.58(12) . . ?
O3 Pb1 O4 60.09(15) . . ?
O3 Pb1 O5 119.01(15) . . ?
O2 Pb1 O6 120.20(14) . . ?
O2 Pb1 O4 119.36(15) . . ?
O2 Pb1 O3 60.94(15) . . ?
O2 Pb1 O5 174.10(12) . . ?
Cl1 Mn1 Cl1 91.82(6) 2_676 . ?
Cl2 Mn1 Cl1 112.54(7) . . ?
Cl2 Mn1 Cl1 110.60(7) . 2_676 ?
Cl2 Mn1 Cl3 115.25(7) . . ?
Cl3 Mn1 Cl1 107.99(7) . . ?
Cl3 Mn1 Cl1 116.28(7) . 2_676 ?
Mn1 Cl1 Mn1 88.19(6) 2_676 . ?
C10 O6 Pb1 118.6(4) . . ?
C10 O6 C11 112.9(5) . . ?
C11 O6 Pb1 112.5(4) . . ?
C12 O1 Pb1 121.3(4) . . ?
C1 O1 Pb1 117.3(4) . . ?
C1 O1 C12 111.3(5) . . ?
C6 O4 Pb1 115.5(4) . . ?
C7 O4 Pb1 114.9(4) . . ?
C7 O4 C6 114.3(6) . . ?
C4 O3 Pb1 116.4(4) . . ?
C5 O3 Pb1 115.9(5) . . ?
C5 O3 C4 112.8(6) . . ?
C8 O5 Pb1 117.0(4) . . ?
C9 O5 Pb1 114.3(4) . . ?
C9 O5 C8 112.0(6) . . ?
C2 O2 Pb1 116.7(4) . . ?
C3 O2 Pb1 115.2(4) . . ?
C3 O2 C2 111.5(6) . . ?
O1 C12 H12A 110.1 . . ?
O1 C12 H12B 110.1 . . ?
O1 C12 C11 108.0(5) . . ?
H12A C12 H12B 108.4 . . ?
C11 C12 H12A 110.1 . . ?
C11 C12 H12B 110.1 . . ?
O6 C10 H10A 110.0 . . ?
O6 C10 H10B 110.0 . . ?
O6 C10 C9 108.5(6) . . ?
H10A C10 H10B 108.4 . . ?
C9 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
O1 C1 H1A 110.2 . . ?
O1 C1 H1B 110.2 . . ?
O1 C1 C2 107.6(6) . . ?
H1A C1 H1B 108.5 . . ?
C2 C1 H1A 110.2 . . ?
C2 C1 H1B 110.2 . . ?
O4 C6 H6A 109.8 . . ?
O4 C6 H6B 109.8 . . ?
O4 C6 C5 109.4(6) . . ?
H6A C6 H6B 108.3 . . ?
C5 C6 H6A 109.8 . . ?
C5 C6 H6B 109.8 . . ?
O3 C4 H4A 109.9 . . ?
O3 C4 H4B 109.9 . . ?
O3 C4 C3 108.7(6) . . ?
H4A C4 H4B 108.3 . . ?
C3 C4 H4A 109.9 . . ?
C3 C4 H4B 109.9 . . ?
O6 C11 C12 107.7(5) . . ?
O6 C11 H11A 110.2 . . ?
O6 C11 H11B 110.2 . . ?
C12 C11 H11A 110.2 . . ?
C12 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
O3 C5 C6 109.2(7) . . ?
O3 C5 H5A 109.8 . . ?
O3 C5 H5B 109.8 . . ?
C6 C5 H5A 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.3 . . ?
O2 C2 C1 108.7(6) . . ?
O2 C2 H2A 109.9 . . ?
O2 C2 H2B 109.9 . . ?
C1 C2 H2A 109.9 . . ?
C1 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
O5 C8 H8A 109.9 . . ?
O5 C8 H8B 109.9 . . ?
O5 C8 C7 108.8(6) . . ?
H8A C8 H8B 108.3 . . ?
C7 C8 H8A 109.9 . . ?
C7 C8 H8B 109.9 . . ?
O5 C9 C10 107.9(6) . . ?
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 . . ?
O4 C7 C8 108.9(6) . . ?
O4 C7 H7A 109.9 . . ?
O4 C7 H7B 109.9 . . ?
C8 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
O2 C3 C4 108.1(7) . . ?
O2 C3 H3A 110.1 . . ?
O2 C3 H3B 110.1 . . ?
C4 C3 H3A 110.1 . . ?
C4 C3 H3B 110.1 . . ?
H3A C3 H3B 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 2.5416(14) . ?
Pb1 O6 2.754(4) . ?
Pb1 O1 2.663(4) . ?
Pb1 O4 2.791(5) . ?
Pb1 O3 2.745(5) . ?
Pb1 O5 2.807(4) . ?
Pb1 O2 2.685(4) . ?
Mn1 Cl1 2.4424(17) . ?
Mn1 Cl1 2.4423(17) 2_676 ?
Mn1 Cl2 2.307(2) . ?
Mn1 Cl3 2.3249(18) . ?
O6 C10 1.420(8) . ?
O6 C11 1.430(8) . ?
O1 C12 1.431(8) . ?
O1 C1 1.421(8) . ?
O4 C6 1.440(9) . ?
O4 C7 1.417(10) . ?
O3 C4 1.439(9) . ?
O3 C5 1.419(10) . ?
O5 C8 1.437(9) . ?
O5 C9 1.414(9) . ?
O2 C2 1.436(8) . ?
O2 C3 1.425(9) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C11 1.483(11) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.488(12) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.482(11) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.455(13) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.479(13) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.474(13) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 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 O6 C10 C9 -42.8(7) . . . . ?
Pb1 O6 C11 C12 56.4(6) . . . . ?
Pb1 O1 C12 C11 35.5(7) . . . . ?
Pb1 O1 C1 C2 -48.8(7) . . . . ?
Pb1 O4 C6 C5 -43.4(8) . . . . ?
Pb1 O4 C7 C8 53.9(7) . . . . ?
Pb1 O3 C4 C3 39.1(8) . . . . ?
Pb1 O3 C5 C6 -51.1(8) . . . . ?
Pb1 O5 C8 C7 41.6(8) . . . . ?
Pb1 O5 C9 C10 -53.0(7) . . . . ?
Pb1 O2 C2 C1 -43.8(7) . . . . ?
Pb1 O2 C3 C4 55.1(7) . . . . ?
O6 C10 C9 O5 62.5(8) . . . . ?
O1 C12 C11 O6 -59.3(7) . . . . ?
O1 C1 C2 O2 59.3(7) . . . . ?
O4 C6 C5 O3 62.0(9) . . . . ?
O3 C4 C3 O2 -61.1(8) . . . . ?
O5 C8 C7 O4 -62.5(8) . . . . ?
C12 O1 C1 C2 165.3(6) . . . . ?
C10 O6 C11 C12 -166.1(6) . . . . ?
C1 O1 C12 C11 179.9(6) . . . . ?
C6 O4 C7 C8 -169.3(6) . . . . ?
C4 O3 C5 C6 171.0(7) . . . . ?
C11 O6 C10 C9 -177.5(6) . . . . ?
C5 O3 C4 C3 176.7(7) . . . . ?
C2 O2 C3 C4 -169.0(6) . . . . ?
C8 O5 C9 C10 171.0(6) . . . . ?
C9 O5 C8 C7 176.3(6) . . . . ?
C7 O4 C6 C5 -179.9(7) . . . . ?
C3 O2 C2 C1 -179.0(6) . . . . ?
