# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

 
data_1

_publ_requested_journal          'Cryst.Growth Des.'
_publ_contact_author_name        'Dr. Natalia V. Pervukhina'
_publ_contact_author_address     
;Nikolaev Institute of Inorganic Chemistry,
SB Russian Academy of Sciences,
Akad. Lavrentiev prospekt 3,
Novosibirsk 90,
630090 Russia
;
_publ_contact_author_email       pervukh@niic.nsc.ru
_publ_contact_author_phone       7(383)3309466
_publ_contact_author_fax         7(383)3309489
loop_
_publ_author_name
_publ_author_address
'Atuchin, V.V.'
;Institute of Semiconductor Physics,
SB Russian Academy of Sciences,
Akad. Lavrentiev prospekt 13,
Novosibirsk 90,
630090 Russia
;
'Ivannikova, N.V.'
;Nikolaev Institute of Inorganic Chemistry,
SB Russian Academy of Sciences,
Akad. Lavrentiev prospekt 3,
Novosibirsk 90,
630090 Russia
;
'Komonov, A.I.'
;Institute of Semiconductor Physics,
SB Russian Academy of Sciences,
Akad. Lavrentiev prospekt 13,
Novosibirsk 90,
630090 Russia
;
'Kuratieva, N.V.'
;Nikolaev Institute of Inorganic Chemistry,
SB Russian Academy of Sciences,
Akad. Lavrentiev prospekt 3,
Novosibirsk 90,
630090 Russia
;
'Loshkarev, I.D.'
;Institute of Semiconductor Physics,
SB Russian Academy of Sciences,
Akad. Lavrentiev prospekt 13,
Novosibirsk 90,
630090 Russia
;
'Pervukhina, Natalia V.'
;Nikolaev Institute of Inorganic Chemistry,
SB Russian Academy of Sciences,
Akad. Lavrentiev prospekt 3,
Novosibirsk 90,
630090 Russia
;
'Pokrovsky, L.D.'
;Institute of Semiconductor Physics,
SB Russian Academy of Sciences,
Akad. Lavrentiev prospekt 13,
Novosibirsk 90,
630090 Russia
;
'Shlegel, V.N.'
;Nikolaev Institute of Inorganic Chemistry,
SB Russian Academy of Sciences,
Akad. Lavrentiev prospekt 3,
Novosibirsk 90,
630090 Russia
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Mo O5 Pb2'
_chemical_formula_sum            'Mo O5 Pb2'
_chemical_formula_weight         590.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mo Mo -1.6832 0.6857 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'

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

_cell_length_a                   14.2221(11)
_cell_length_b                   5.7852(5)
_cell_length_c                   7.3262(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.168(2)
_cell_angle_gamma                90.00
_cell_volume                     549.95(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1873
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      32.55

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    7.130
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             984
_exptl_absorpt_coefficient_mu    63.251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.031
_exptl_absorpt_correction_T_max  0.282
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean 25
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            2753
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         32.57
_reflns_number_total             1089
_reflns_number_gt                1015
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_cell_refinement       'SAINT (Bruker, 2011)'
_computing_data_reduction        'SAINT (Bruker, 2011)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'local program'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0534P)²+47.6229P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1089
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0851
_refine_ls_wR_factor_gt          0.0834
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.000
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.13713(2) 0.0000 0.11447(5) 0.01225(12) Uani 1 2 d S . .
Pb2 Pb 0.01350(3) 0.5000 0.25628(4) 0.01035(11) Uani 1 2 d S . .
Mo1 Mo 0.33103(6) 0.5000 0.34061(11) 0.00918(15) Uani 1 2 d S . .
O1 O 0.0859(6) 0.0000 0.3999(10) 0.0237(15) Uani 1 2 d S . .
O2 O 0.3528(4) 0.7425(9) 0.2182(8) 0.0232(10) Uani 1 1 d . . .
O3 O 0.2009(6) 0.5000 0.3069(13) 0.0269(16) Uani 1 2 d S . .
O4 O 0.0000 0.2550(9) 0.0000 0.0110(10) Uani 1 2 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.00939(17) 0.01268(17) 0.01437(18) 0.000 0.00454(13) 0.000
Pb2 0.01129(19) 0.01146(17) 0.00936(17) 0.000 0.00530(13) 0.000
Mo1 0.0073(3) 0.0097(3) 0.0112(3) 0.000 0.0045(2) 0.000
O1 0.019(3) 0.033(4) 0.013(3) 0.000 0.001(3) 0.000
O2 0.021(2) 0.017(2) 0.030(2) 0.0091(19) 0.008(2) 0.000(2)
O3 0.015(3) 0.032(4) 0.037(4) 0.000 0.014(3) 0.000
O4 0.014(3) 0.010(2) 0.011(2) 0.000 0.006(2) 0.000

_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 O4 2.312(3) 5 ?
Pb1 O4 2.312(3) . ?
Pb1 O1 2.480(7) . ?
Pb1 Pb1 3.5597(7) 5 ?
Pb2 O4 2.297(3) . ?
Pb2 O4 2.297(3) 5_565 ?
Pb2 O3 2.536(8) . ?
Pb2 O2 2.645(5) 3_445 ?
Pb2 O2 2.645(5) 8_465 ?
Pb2 Pb2 3.6149(7) 5_565 ?
Mo1 O2 1.759(5) 6_565 ?
Mo1 O2 1.759(5) . ?
Mo1 O3 1.764(8) . ?
Mo1 O1 1.781(7) 7_556 ?
O1 Mo1 1.781(7) 7_556 ?
O2 Pb2 2.645(5) 3 ?
O4 Pb2 2.297(3) 5_565 ?
O4 Pb1 2.312(3) 5 ?


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
O4 Pb1 O4 79.3(2) 5 . ?
O4 Pb1 O1 79.07(13) 5 . ?
O4 Pb1 O1 79.07(13) . . ?
O4 Pb1 Pb1 39.66(10) 5 5 ?
O4 Pb1 Pb1 39.66(10) . 5 ?
O1 Pb1 Pb1 75.75(16) . 5 ?
O4 Pb2 O4 76.2(2) . 5_565 ?
O4 Pb2 O3 81.41(15) . . ?
O4 Pb2 O3 81.41(15) 5_565 . ?
O4 Pb2 O2 77.69(13) . 3_445 ?
O4 Pb2 O2 118.80(12) 5_565 3_445 ?
O3 Pb2 O2 145.71(11) . 3_445 ?
O4 Pb2 O2 118.80(12) . 8_465 ?
O4 Pb2 O2 77.69(13) 5_565 8_465 ?
O3 Pb2 O2 145.71(11) . 8_465 ?
O2 Pb2 O2 68.6(2) 3_445 8_465 ?
O4 Pb2 Pb2 38.10(11) . 5_565 ?
O4 Pb2 Pb2 38.10(11) 5_565 5_565 ?
O3 Pb2 Pb2 79.1(2) . 5_565 ?
O2 Pb2 Pb2 99.83(12) 3_445 5_565 ?
O2 Pb2 Pb2 99.83(12) 8_465 5_565 ?
O2 Mo1 O2 105.7(4) 6_565 . ?
O2 Mo1 O3 108.8(2) 6_565 . ?
O2 Mo1 O3 108.8(2) . . ?
O2 Mo1 O1 111.5(2) 6_565 7_556 ?
O2 Mo1 O1 111.5(2) . 7_556 ?
O3 Mo1 O1 110.4(4) . 7_556 ?
Mo1 O1 Pb1 127.2(4) 7_556 . ?
Mo1 O2 Pb2 136.1(3) . 3 ?
Mo1 O3 Pb2 179.7(5) . . ?
Pb2 O4 Pb2 103.8(2) . 5_565 ?
Pb2 O4 Pb1 117.782(13) . 5 ?
Pb2 O4 Pb1 108.751(11) 5_565 5 ?
Pb2 O4 Pb1 108.751(11) . . ?
Pb2 O4 Pb1 117.782(13) 5_565 . ?
Pb1 O4 Pb1 100.7(2) 5 . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         5.415
_refine_diff_density_min         -6.071
_refine_diff_density_rms         0.672

# start Validation Reply Form
_vrf_PLAT971_I                   
;
PROBLEM: Check Calcd Residual Density  0.97A From     Pb1       5.17 eA-3  
RESPONSE: All problems with the residual dencity causes the heavy metal atom 
inside the composition. The value of residual dencity peaks do not exceed the 
1/10 of heavy Pb (atomic number 82).
;
_vrf_PLAT972_I                   
;
PROBLEM: Check Calcd Residual Density  0.73A From     Pb2      -5.96 eA-3  
RESPONSE: All problems with the residual dencity causes the heavy metal atom 
inside the composition. The value of residual dencity peaks do not exceed the 
1/10 of heavy Pb (atomic number 82).
;

# end Validation Reply Form
