# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PbMn3(CO)18ALCl4
_database_code_depnum_ccdc_archive 'CCDC 1890307'
loop_
_audit_author_name
_audit_author_address
'Silke Wolf'
;Karlsruher Institut f?r Technologie
Germany
;
_audit_update_record             
;
2019-01-11 deposited with the CCDC.	2019-03-11 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 Al Cl4 Mn3 O15 Pb'
_chemical_formula_weight         960.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.1771 0.1873 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3281 0.5435 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.0162 2.2332 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.4950 6.8412 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.208(2)
_cell_length_b                   17.620(3)
_cell_length_c                   17.915(5)
_cell_angle_alpha                90
_cell_angle_beta                 120.94(2)
_cell_angle_gamma                90
_cell_volume                     2763.8(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    150
_cell_measurement_reflns_used    36899
_cell_measurement_theta_min      3.32
_cell_measurement_theta_max      64.34

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.309
_exptl_crystal_F_000             1792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    18.302
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0010
_exptl_absorpt_correction_T_max  0.0063
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150
_diffrn_radiation_wavelength     1.34143
_diffrn_radiation_type           GaK\a
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_source                   'Metaljet D2'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_detector                 EIGER4M
_diffrn_detector_area_resol_mean 13.33
_diffrn_reflns_number            17096
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.320
_diffrn_reflns_theta_max         62.547
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measured_fraction_theta_full 0.846
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_Laue_measured_fraction_full 0.846
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_point_group_measured_fraction_full 0.846
_reflns_number_total             6331
_reflns_number_gt                5895
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0605P)²+4.7900P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6331
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0889
_refine_ls_wR_factor_gt          0.0876
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.998
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 -0.18600(2) -0.27485(2) -0.09871(2) 0.02995(7) Uani 1 1 d . . . . .
Mn1 Mn -0.22490(7) -0.14302(3) -0.02925(4) 0.03406(14) Uani 1 1 d . . . . .
C1 C -0.3374(5) -0.1932(2) 0.0112(3) 0.0422(9) Uani 1 1 d . . . . .
O1 O -0.4099(5) -0.2173(2) 0.0368(3) 0.0550(9) Uani 1 1 d . . . . .
C2 C -0.3993(5) -0.1291(2) -0.1378(3) 0.0416(9) Uani 1 1 d . . . . .
O2 O -0.5049(4) -0.1190(2) -0.2036(2) 0.0554(9) Uani 1 1 d . . . . .
C3 C -0.1095(5) -0.0899(2) -0.0662(3) 0.0369(8) Uani 1 1 d . . . . .
O3 O -0.0383(4) -0.05472(18) -0.0839(2) 0.0443(7) Uani 1 1 d . . . . .
C4 C -0.0395(6) -0.1696(3) 0.0694(3) 0.0426(9) Uani 1 1 d . . . . .
O4 O 0.0777(4) -0.1848(2) 0.1254(2) 0.0553(9) Uani 1 1 d . . . . .
C5 C -0.2598(6) -0.0545(3) 0.0131(3) 0.0452(10) Uani 1 1 d . . . . .
O5 O -0.2889(5) -0.0006(2) 0.0360(3) 0.0604(9) Uani 1 1 d . . . . .
Mn2 Mn -0.43817(7) -0.35950(3) -0.21772(4) 0.03287(13) Uani 1 1 d . . . . .
C6 C -0.5427(5) -0.3156(3) -0.1693(3) 0.0422(9) Uani 1 1 d . . . . .
O6 O -0.6097(5) -0.2869(2) -0.1426(3) 0.0557(9) Uani 1 1 d . . . . .
C7 C -0.5043(5) -0.2798(2) -0.2966(3) 0.0362(8) Uani 1 1 d . . . . .
O7 O -0.5538(4) -0.23474(18) -0.3484(2) 0.0445(7) Uani 1 1 d . . . . .
C8 C -0.3161(5) -0.3918(2) -0.2610(3) 0.0414(9) Uani 1 1 d . . . . .
O8 O -0.2471(4) -0.4102(2) -0.2905(2) 0.0554(8) Uani 1 1 d . . . . .
C9 C -0.3703(5) -0.4398(3) -0.1372(3) 0.0440(10) Uani 1 1 d . . . . .
O9 O -0.3358(5) -0.4902(2) -0.0926(3) 0.0589(9) Uani 1 1 d . . . . .
C10 C -0.5990(5) -0.4165(3) -0.2973(3) 0.0428(9) Uani 1 1 d . . . . .
O10 O -0.6982(4) -0.4512(2) -0.3493(2) 0.0554(9) Uani 1 1 d . . . . .
Mn3 Mn 0.09893(7) -0.32833(3) -0.05264(4) 0.03152(13) Uani 1 1 d . . . . .
C11 C 0.1459(5) -0.3418(3) 0.0617(3) 0.0395(9) Uani 1 1 d . . . . .
O11 O 0.1851(4) -0.3522(2) 0.1317(2) 0.0542(9) Uani 1 1 d . . . . .
C12 C 0.1664(5) -0.2283(2) -0.0264(3) 0.0371(9) Uani 1 1 d . . . . .
O12 O 0.2134(4) -0.16911(18) -0.0075(2) 0.0482(7) Uani 1 1 d . . . . .
C13 C 0.0491(5) -0.3150(2) -0.1673(3) 0.0402(9) Uani 1 1 d . . . . .
O13 O 0.0239(5) -0.3082(2) -0.2358(2) 0.0545(8) Uani 1 1 d . . . . .
C14 C 0.0120(5) -0.4240(2) -0.0796(3) 0.0384(8) Uani 1 1 d . . . . .
O14 O -0.0421(4) -0.48239(19) -0.0960(2) 0.0504(8) Uani 1 1 d . . . . .
C15 C 0.2918(5) -0.3643(2) -0.0211(3) 0.0394(9) Uani 1 1 d . . . . .
O15 O 0.4096(4) -0.3851(2) 0.0004(3) 0.0517(8) Uani 1 1 d . . . . .
Al1 Al -0.11193(16) -0.39873(7) 0.19871(8) 0.0380(3) Uani 1 1 d . . . . .
Cl1 Cl -0.17883(13) -0.36269(6) 0.06884(7) 0.0438(2) Uani 1 1 d . . . . .
Cl2 Cl -0.21956(13) -0.32222(6) 0.24543(7) 0.0444(2) Uani 1 1 d . . . . .
Cl3 Cl 0.12568(15) -0.39180(10) 0.28471(8) 0.0615(3) Uani 1 1 d . . . . .
Cl4 Cl -0.1987(2) -0.50947(7) 0.19275(11) 0.0719(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 Mn3 2.7497(8) . ?
Pb1 Mn1 2.7585(7) . ?
Pb1 Mn2 2.7845(9) . ?
Mn1 C5 1.848(5) . ?
Mn1 C2 1.858(5) . ?
Mn1 C1 1.866(5) . ?
Mn1 C4 1.867(5) . ?
Mn1 C3 1.872(4) . ?
C1 O1 1.134(6) . ?
C2 O2 1.129(6) . ?
C3 O3 1.118(5) . ?
C4 O4 1.129(6) . ?
C5 O5 1.133(6) . ?
Mn2 C10 1.825(5) . ?
Mn2 C7 1.855(4) . ?
Mn2 C6 1.854(5) . ?
Mn2 C8 1.864(5) . ?
Mn2 C9 1.880(5) . ?
C6 O6 1.136(6) . ?
C7 O7 1.125(5) . ?
C8 O8 1.123(6) . ?
C9 O9 1.122(6) . ?
C10 O10 1.139(6) . ?
Mn3 C14 1.850(5) . ?
Mn3 C13 1.861(4) . ?
Mn3 C15 1.858(4) . ?
Mn3 C12 1.863(4) . ?
Mn3 C11 1.863(4) . ?
C11 O11 1.119(6) . ?
C12 O12 1.124(5) . ?
C13 O13 1.123(6) . ?
C14 O14 1.133(6) . ?
C15 O15 1.120(5) . ?
Al1 Cl3 2.105(2) . ?
Al1 Cl4 2.1227(18) . ?
Al1 Cl1 2.1562(17) . ?
Al1 Cl2 2.1612(16) . ?

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
Mn3 Pb1 Mn1 121.91(2) . . ?
Mn3 Pb1 Mn2 117.71(2) . . ?
Mn1 Pb1 Mn2 120.38(2) . . ?
C5 Mn1 C2 92.0(2) . . ?
C5 Mn1 C1 87.3(2) . . ?
C2 Mn1 C1 91.1(2) . . ?
C5 Mn1 C4 98.0(2) . . ?
C2 Mn1 C4 169.6(2) . . ?
C1 Mn1 C4 92.3(2) . . ?
C5 Mn1 C3 90.75(19) . . ?
C2 Mn1 C3 90.12(19) . . ?
C1 Mn1 C3 177.74(19) . . ?
C4 Mn1 C3 86.81(19) . . ?
C5 Mn1 Pb1 177.44(17) . . ?
C2 Mn1 Pb1 85.53(14) . . ?
C1 Mn1 Pb1 92.09(13) . . ?
C4 Mn1 Pb1 84.54(14) . . ?
C3 Mn1 Pb1 89.90(12) . . ?
O1 C1 Mn1 173.8(4) . . ?
O2 C2 Mn1 178.5(4) . . ?
O3 C3 Mn1 175.2(4) . . ?
O4 C4 Mn1 174.7(4) . . ?
O5 C5 Mn1 176.5(5) . . ?
C10 Mn2 C7 89.61(19) . . ?
C10 Mn2 C6 95.3(2) . . ?
C7 Mn2 C6 88.2(2) . . ?
C10 Mn2 C8 91.8(2) . . ?
C7 Mn2 C8 88.48(19) . . ?
C6 Mn2 C8 172.1(2) . . ?
C10 Mn2 C9 90.8(2) . . ?
C7 Mn2 C9 179.6(2) . . ?
C6 Mn2 C9 91.6(2) . . ?
C8 Mn2 C9 91.6(2) . . ?
C10 Mn2 Pb1 177.81(16) . . ?
C7 Mn2 Pb1 90.51(13) . . ?
C6 Mn2 Pb1 86.92(14) . . ?
C8 Mn2 Pb1 85.97(14) . . ?
C9 Mn2 Pb1 89.13(14) . . ?
O6 C6 Mn2 177.2(4) . . ?
O7 C7 Mn2 174.8(4) . . ?
O8 C8 Mn2 177.1(4) . . ?
O9 C9 Mn2 176.2(4) . . ?
O10 C10 Mn2 177.4(4) . . ?
C14 Mn3 C13 90.26(19) . . ?
C14 Mn3 C15 93.44(19) . . ?
C13 Mn3 C15 91.4(2) . . ?
C14 Mn3 C12 173.61(19) . . ?
C13 Mn3 C12 90.86(19) . . ?
C15 Mn3 C12 92.82(19) . . ?
C14 Mn3 C11 89.37(19) . . ?
C13 Mn3 C11 179.2(2) . . ?
C15 Mn3 C11 89.35(19) . . ?
C12 Mn3 C11 89.42(19) . . ?
C14 Mn3 Pb1 86.70(13) . . ?
C13 Mn3 Pb1 88.80(14) . . ?
C15 Mn3 Pb1 179.77(16) . . ?
C12 Mn3 Pb1 87.04(14) . . ?
C11 Mn3 Pb1 90.46(14) . . ?
O11 C11 Mn3 174.4(4) . . ?
O12 C12 Mn3 176.8(4) . . ?
O13 C13 Mn3 177.5(4) . . ?
O14 C14 Mn3 179.4(4) . . ?
O15 C15 Mn3 177.9(4) . . ?
Cl3 Al1 Cl4 112.59(9) . . ?
Cl3 Al1 Cl1 112.29(8) . . ?
Cl4 Al1 Cl1 108.90(8) . . ?
Cl3 Al1 Cl2 107.72(8) . . ?
Cl4 Al1 Cl2 108.12(7) . . ?
Cl1 Al1 Cl2 106.99(7) . . ?



_refine_diff_density_max         3.226
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.153

_shelxl_version_number           2013-2


_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
