# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1879545'
loop_
_audit_author_name
_audit_author_address
'Conggang Li'
;State Key Laboratory of Crystal Materials & Institute of Crystal Materials, Shandong University
China
;
_audit_update_record             
;
2018-11-17 deposited with the CCDC.	2019-02-26 downloaded from the CCDC.
;
_audit_creation_date             2018-09-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(Bi12 Fe4 Mo8 O48)'
_chemical_formula_sum            'Bi3 Fe Mo2 O12'
_chemical_formula_weight         1066.67
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.927(12)
_cell_length_b                   11.672(12)
_cell_length_c                   5.263(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.160(10)
_cell_angle_gamma                90
_cell_volume                     993.6(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1317
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      4.16
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    56.876
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1113 before and 0.0540 after correction.
The Ratio of minimum to maximum transmission is 0.3857.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    7.131
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0915
_diffrn_reflns_av_unetI/netI     0.0927
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2782
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.498
_diffrn_reflns_theta_min         2.152
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                827
_reflns_number_total             1016
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         4.421
_refine_diff_density_min         -2.976
_refine_diff_density_rms         0.836
_refine_ls_extinction_coef       0.0067(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1016
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0482
_refine_ls_restrained_S_all      0.984
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0673P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1254
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
O2 \\sim O1 \\sim O3 \\sim O6 \\sim O4 \\sim O5: within 3.8A with sigma of 0.01
and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O6) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Bi2 Bi 0.34846(5) 0.38680(6) 0.59387(12) 0.0081(3) Uani 1 1 d . . . . .
Bi1 Bi 0.500000 0.84480(9) 1.250000 0.0088(4) Uani 1 2 d S T P . .
Mo1 Mo 0.16815(11) 0.62776(14) 0.4237(3) 0.0089(5) Uani 1 1 d . . . . .
Fe1 Fe 0.500000 0.6176(3) 0.750000 0.0079(9) Uani 1 2 d S T P . .
O2 O 0.4128(9) 0.5400(12) 0.494(2) 0.013(2) Uani 1 1 d . U . . .
O1 O 0.4497(8) 0.7033(11) 0.973(2) 0.013(3) Uani 1 1 d . U . . .
O3 O 0.2469(9) 0.5415(12) 0.635(2) 0.013(2) Uani 1 1 d . U . . .
O6 O 0.0917(9) 0.5462(12) 0.197(2) 0.013(2) Uani 1 1 d . U . . .
O4 O 0.2171(8) 0.7132(12) 0.235(2) 0.013(2) Uani 1 1 d . U . . .
O5 O 0.1153(8) 0.7107(12) 0.618(2) 0.012(2) Uani 1 1 d . U . . .

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
Bi2 0.0153(5) 0.0019(5) 0.0070(4) -0.0002(2) 0.0033(3) 0.0000(3)
Bi1 0.0175(7) 0.0014(6) 0.0082(5) 0.000 0.0049(4) 0.000
Mo1 0.0146(10) 0.0051(10) 0.0078(9) 0.0002(6) 0.0043(7) 0.0016(7)
Fe1 0.010(2) 0.005(2) 0.0084(19) 0.000 0.0017(16) 0.000
O2 0.019(4) 0.008(4) 0.012(4) -0.002(3) 0.004(3) 0.001(3)
O1 0.017(4) 0.007(4) 0.015(4) -0.004(4) 0.006(4) -0.002(4)
O3 0.017(4) 0.009(4) 0.012(3) 0.000(3) 0.004(3) 0.000(3)
O6 0.019(4) 0.009(4) 0.012(4) -0.002(3) 0.005(3) -0.001(3)
O4 0.021(5) 0.010(5) 0.010(4) -0.001(4) 0.006(4) 0.002(4)
O5 0.016(5) 0.009(5) 0.014(4) -0.002(4) 0.010(4) 0.002(4)

_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
Bi2 Bi1 3.649(3) 5_667 ?
Bi2 O2 2.235(12) 6_566 ?
Bi2 O2 2.236(14) . ?
Bi2 O1 2.257(14) 6_565 ?
Bi2 O3 2.652(12) 6_565 ?
Bi2 O3 2.546(14) . ?
Bi2 O4 2.683(13) 4_545 ?
Bi2 O5 2.519(14) 4_546 ?
Bi1 O1 2.202(13) 2_657 ?
Bi1 O1 2.202(13) . ?
Bi1 O6 2.722(12) 8_567 ?
Bi1 O6 2.722(12) 7_566 ?
Bi1 O5 2.346(14) 8_566 ?
Bi1 O5 2.346(14) 7_567 ?
Mo1 O3 1.776(13) . ?
Mo1 O6 1.758(13) . ?
Mo1 O4 1.775(14) . ?
Mo1 O5 1.825(14) . ?
Fe1 O2 1.908(13) 2_656 ?
Fe1 O2 1.908(13) . ?
Fe1 O1 1.920(14) . ?
Fe1 O1 1.920(14) 2_656 ?

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
O2 Bi2 Bi1 106.6(4) . 5_667 ?
O2 Bi2 Bi1 87.5(4) 6_566 5_667 ?
O2 Bi2 O2 77.3(3) 6_566 . ?
O2 Bi2 O1 80.9(5) . 6_565 ?
O2 Bi2 O1 104.1(5) 6_566 6_565 ?
O2 Bi2 O3 137.9(4) 6_566 6_565 ?
O2 Bi2 O3 80.9(5) . . ?
O2 Bi2 O3 76.3(5) . 6_565 ?
O2 Bi2 O3 78.6(5) 6_566 . ?
O2 Bi2 O4 126.1(4) . 4_545 ?
O2 Bi2 O4 152.9(5) 6_566 4_545 ?
O2 Bi2 O5 77.4(4) 6_566 4_546 ?
O2 Bi2 O5 138.1(4) . 4_546 ?
O1 Bi2 Bi1 34.6(3) 6_565 5_667 ?
O1 Bi2 O3 160.5(5) 6_565 . ?
O1 Bi2 O3 103.4(4) 6_565 6_565 ?
O1 Bi2 O4 70.7(4) 6_565 4_545 ?
O1 Bi2 O5 73.7(5) 6_565 4_546 ?
O3 Bi2 Bi1 162.4(3) . 5_667 ?
O3 Bi2 Bi1 131.5(3) 6_565 5_667 ?
O3 Bi2 O3 65.2(3) . 6_565 ?
O3 Bi2 O4 67.5(4) 6_565 4_545 ?
O3 Bi2 O4 115.4(4) . 4_545 ?
O4 Bi2 Bi1 73.4(3) 4_545 5_667 ?
O5 Bi2 Bi1 39.6(3) 4_546 5_667 ?
O5 Bi2 O3 125.3(4) 4_546 . ?
O5 Bi2 O3 141.5(4) 4_546 6_565 ?
O5 Bi2 O4 75.7(4) 4_546 4_545 ?
Bi2 Bi1 Bi2 84.42(8) 6_566 5_667 ?
O1 Bi1 Bi2 35.6(4) 2_657 5_667 ?
O1 Bi1 Bi2 35.6(4) . 6_566 ?
O1 Bi1 Bi2 72.7(4) . 5_667 ?
O1 Bi1 Bi2 72.7(4) 2_657 6_566 ?
O1 Bi1 O1 82.8(7) . 2_657 ?
O1 Bi1 O6 159.0(4) . 8_567 ?
O1 Bi1 O6 159.0(4) 2_657 7_566 ?
O1 Bi1 O6 76.5(4) . 7_566 ?
O1 Bi1 O6 76.5(4) 2_657 8_567 ?
O1 Bi1 O5 78.2(5) . 7_567 ?
O1 Bi1 O5 77.9(5) . 8_566 ?
O1 Bi1 O5 78.2(5) 2_657 8_566 ?
O1 Bi1 O5 77.9(5) 2_657 7_567 ?
O6 Bi1 Bi2 88.2(3) 7_566 6_566 ?
O6 Bi1 Bi2 136.4(3) 8_567 6_566 ?
O6 Bi1 Bi2 88.2(3) 8_567 5_667 ?
O6 Bi1 Bi2 136.4(3) 7_566 5_667 ?
O6 Bi1 O6 124.3(6) 8_567 7_566 ?
O5 Bi1 Bi2 108.6(3) 8_566 6_566 ?
O5 Bi1 Bi2 108.6(3) 7_567 5_667 ?
O5 Bi1 Bi2 43.2(3) 8_566 5_667 ?
O5 Bi1 Bi2 43.2(3) 7_567 6_566 ?
O5 Bi1 O6 94.2(4) 8_566 8_567 ?
O5 Bi1 O6 94.2(4) 7_567 7_566 ?
O5 Bi1 O6 100.7(4) 8_566 7_566 ?
O5 Bi1 O6 100.7(4) 7_567 8_567 ?
O5 Bi1 O5 147.9(7) 7_567 8_566 ?
O3 Mo1 O5 110.5(6) . . ?
O6 Mo1 O3 112.6(6) . . ?
O6 Mo1 O4 107.2(6) . . ?
O6 Mo1 O5 106.5(7) . . ?
O4 Mo1 O3 106.4(7) . . ?
O4 Mo1 O5 113.8(7) . . ?
O2 Fe1 O2 123.3(8) 2_656 . ?
O2 Fe1 O1 106.8(6) 2_656 2_656 ?
O2 Fe1 O1 106.8(6) . . ?
O2 Fe1 O1 101.9(5) 2_656 . ?
O2 Fe1 O1 101.9(5) . 2_656 ?
O1 Fe1 O1 117.2(8) . 2_656 ?
Bi2 O2 Bi2 113.0(6) 6_565 . ?
Fe1 O2 Bi2 122.8(6) . . ?
Fe1 O2 Bi2 123.0(7) . 6_565 ?
Bi1 O1 Bi2 109.8(6) . 6_566 ?
Fe1 O1 Bi2 116.1(6) . 6_566 ?
Fe1 O1 Bi1 129.9(7) . . ?
Bi2 O3 Bi2 91.7(4) . 6_566 ?
Mo1 O3 Bi2 123.8(7) . 6_566 ?
Mo1 O3 Bi2 138.5(6) . . ?
Mo1 O6 Bi1 116.8(6) . 7_566 ?
Mo1 O4 Bi2 127.8(7) . 4 ?
Bi1 O5 Bi2 97.1(5) 7_567 4_556 ?
Mo1 O5 Bi2 134.3(7) . 4_556 ?
Mo1 O5 Bi1 127.4(7) . 7_567 ?

_shelx_res_file                  
;
TITL 1_a.res in C2/c
    1.res
    created by SHELXL-2017/1 at 10:19:49 on 15-Sep-2018
REM Old TITL 1 in C2/c #15
REM SHELXT solution in C2/c
REM R1 0.130, Rweak 0.009, Alpha 0.055, Orientation as input
REM Formula found by SHELXT: O10 Fe Mo2 Bi3
CELL 0.71073 16.9271 11.672 5.2633 90 107.16 90
ZERR 4 0.0117 0.0117 0.0043 0 0.01 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC Bi Fe Mo O
UNIT 12 4 8 48
SIMU 0.01 0.02 3.8 $O
ISOR 0.005 0.01 O1 O2 O3 O6

L.S. 12
PLAN  20
TEMP 23
BOND $H
LIST 6
fmap 2
acta
OMIT -2 53
OMIT -19 3 2
REM <olex2.extras>
REM <HklSrc "%.\\1.hkl">
REM </olex2.extras>

WGHT    0.067300
EXTI    0.006681
FVAR       0.14597
BI2   1    0.348464    0.386798    0.593872    11.00000    0.01529    0.00194 =
         0.00705   -0.00017    0.00334    0.00001
BI1   1    0.500000    0.844798    1.250000    10.50000    0.01750    0.00143 =
         0.00819    0.00000    0.00489    0.00000
MO1   3    0.168145    0.627757    0.423737    11.00000    0.01458    0.00508 =
         0.00776    0.00017    0.00428    0.00160
FE1   2    0.500000    0.617580    0.750000    10.50000    0.00953    0.00533 =
         0.00836    0.00000    0.00172    0.00000
O2    4    0.412845    0.539990    0.493843    11.00000    0.01862    0.00762 =
         0.01201   -0.00237    0.00388    0.00051
O1    4    0.449713    0.703266    0.972738    11.00000    0.01713    0.00714 =
         0.01479   -0.00387    0.00618   -0.00191
O3    4    0.246889    0.541476    0.635313    11.00000    0.01718    0.00896 =
         0.01243    0.00030    0.00421    0.00017
O6    4    0.091704    0.546241    0.197099    11.00000    0.01875    0.00923 =
         0.01218   -0.00162    0.00546   -0.00134
O4    4    0.217060    0.713161    0.234929    11.00000    0.02085    0.00997 =
         0.01038   -0.00082    0.00597    0.00180
O5    4    0.115285    0.710747    0.618451    11.00000    0.01626    0.00892 =
         0.01385   -0.00195    0.01017    0.00231
HKLF 4




REM  1_a.res in C2/c
REM R1 =  0.0482 for     827 Fo > 4sig(Fo)  and  0.0584 for all    1016 data
REM     84 parameters refined using     78 restraints

END

WGHT      0.0673      0.0000

REM Highest difference peak  4.421,  deepest hole -2.976,  1-sigma level  0.836
Q1    1   0.2994  0.3491  0.6194  11.00000  0.05    4.42
Q2    1   0.2936  0.4150  0.6008  11.00000  0.05    4.25
Q3    1   0.3057  0.3834  0.4675  11.00000  0.05    3.74
Q4    1   0.4573  0.8554  1.1203  11.00000  0.05    3.71
Q5    1   0.5000  0.9439  1.2500  10.50000  0.05    3.59
Q6    1   0.5542  0.8219  1.2418  11.00000  0.05    3.48
Q7    1   0.1182  0.6258  0.4249  11.00000  0.05    3.00
Q8    1   0.3930  0.3556  0.5742  11.00000  0.05    2.97
Q9    1   0.5395  0.8816  1.2182  11.00000  0.05    2.89
Q10   1   0.5391  0.6508  0.8852  11.00000  0.05    2.86
Q11   1   0.3616  0.2980  0.5536  11.00000  0.05    2.80
Q12   1   0.1279  0.6263  0.2729  11.00000  0.05    2.71
Q13   1   0.4701  0.6615  0.8067  11.00000  0.05    2.61
Q14   1   0.3609  0.4812  0.5928  11.00000  0.05    2.53
Q15   1   0.3768  0.3875  0.7188  11.00000  0.05    2.53
Q16   1   0.3499  0.3674  0.3219  11.00000  0.05    2.50
Q17   1   0.4647  0.5822  0.7710  11.00000  0.05    2.36
Q18   1   0.2027  0.6211  0.5684  11.00000  0.05    2.31
Q19   1   0.4624  0.5675  0.6103  11.00000  0.05    2.24
Q20   1   0.4879  0.8365  0.9555  11.00000  0.05    2.04
;
_shelx_res_checksum              6007
_shelx_SHELXL_version_number     2017/1
_olex2_submission_special_instructions 'No special instructions were received'
