# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 1430700'
_audit_update_record             
;
2015-10-11 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            CMF-1
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Cu6 Mo28 N2 O96'
_chemical_formula_weight         4631.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I 4/m '

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

_cell_length_a                   17.2929(7)
_cell_length_b                   17.2929(7)
_cell_length_c                   19.8829(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5945.9(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    180.0(2)
_cell_measurement_reflns_used    1821
_cell_measurement_theta_min      3.2819
_cell_measurement_theta_max      29.8313

_exptl_crystal_description       blackblock
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4264
_exptl_absorpt_coefficient_mu    3.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5035
_exptl_absorpt_correction_T_max  0.7415
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.6 (release 27-01-2011 CrysAlis171 .NET)
(compiled Jan 27 2011,13:34:29)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      180.0(2)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.3914
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3014
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         26.02
_reflns_number_total             3014
_reflns_number_gt                2199
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.6 (release 27-01-2011 CrysAlis171 .NET)
(compiled Jan 27 2011,13:34:29)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.6 (release 27-01-2011 CrysAlis171 .NET)
(compiled Jan 27 2011,13:34:29)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.6 (release 27-01-2011 CrysAlis171 .NET)
(compiled Jan 27 2011,13:34:29)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0478P)²+3.4382P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   CONSTR
_refine_ls_hydrogen_treatment    CONSTR
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3014
_refine_ls_number_parameters     100
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.1081
_refine_ls_wR_factor_gt          0.1012
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.62243(4) 0.10180(4) 0.0000 0.0168(2) Uani 1 2 d S . .
Mo2 Mo 0.77920(3) 0.02927(3) 0.08218(3) 0.01930(17) Uani 1 1 d . . .
Mo3 Mo 0.64977(4) 0.11036(3) 0.17037(3) 0.02587(18) Uani 1 1 d . . .
Mo4 Mo 0.69951(4) 0.25734(3) 0.08222(3) 0.02352(18) Uani 1 1 d . . .
Cu1 Cu 0.0000 0.0000 0.0000 0.0534(9) Uani 1 8 d S . .
Cu2 Cu 0.81820(8) -0.14381(7) 0.0000 0.0326(3) Uani 1 2 d S . .
Cu3 Cu 0.5000 0.0000 0.2500 0.0508(11) Uani 0.50 4 d SP . .
O1 O 0.7103(3) 0.1315(3) 0.2354(2) 0.0385(12) Uiso 1 1 d . . .
O2 O 0.6533(3) 0.3442(3) 0.0736(2) 0.0381(13) Uiso 1 1 d . . .
O3 O 0.7748(3) 0.2755(3) 0.1347(2) 0.0361(12) Uiso 1 1 d . . .
O4 O 0.7985(3) -0.0688(3) 0.0732(2) 0.0295(11) Uiso 1 1 d . . .
O5 O 0.7632(3) 0.2563(3) 0.0000 0.0202(14) Uiso 1 2 d S . .
O6 O 0.6893(3) 0.0165(3) 0.0000 0.0189(13) Uiso 1 2 d S . .
O7 O 0.5663(3) 0.0829(3) 0.0701(2) 0.0283(11) Uiso 1 1 d . . .
O8 O 0.5644(3) 0.0829(3) 0.2081(2) 0.0377(12) Uiso 1 1 d . . .
O9 O 0.8459(3) 0.0618(3) 0.1383(2) 0.0313(11) Uiso 1 1 d . . .
O10 O 0.6920(3) 0.0127(3) 0.1441(2) 0.0257(11) Uiso 1 1 d . . .
O11 O 0.8283(3) 0.0657(3) 0.0000 0.0206(14) Uiso 1 2 d S . .
O12 O 0.6233(3) 0.2148(3) 0.1447(2) 0.0311(11) Uiso 1 1 d . . .
O13 O 0.6245(3) 0.2110(3) 0.0000 0.0228(14) Uiso 1 2 d S . .
O14 O 0.7132(2) 0.1329(2) 0.08103(19) 0.0189(9) Uiso 1 1 d . . .
N1 N 0.0000 0.0000 0.0951(8) 0.055(4) Uani 1 4 d S . .


_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
Mo1 O7 1.730(4) 10 ?
Mo1 O7 1.730(4) . ?
Mo1 O6 1.875(6) . ?
Mo1 O13 1.889(6) . ?
Mo1 O14 2.313(4) . ?
Mo1 O14 2.313(4) 10 ?
Mo2 O9 1.701(5) . ?
Mo2 O4 1.737(5) . ?
Mo2 O11 1.946(3) . ?
Mo2 O10 1.968(4) . ?
Mo2 O14 2.125(4) . ?
Mo2 O6 2.266(4) . ?
Mo2 Mo3 3.1703(8) . ?
Mo3 O1 1.703(5) . ?
Mo3 O8 1.723(5) . ?
Mo3 O10 1.913(4) . ?
Mo3 O12 1.932(5) . ?
Mo3 O14 2.124(4) . ?
Mo3 O7 2.507(5) . ?
Mo3 Mo4 3.2050(8) . ?
Mo4 O3 1.698(5) . ?
Mo4 O2 1.710(5) . ?
Mo4 O12 1.955(5) . ?
Mo4 O5 1.971(3) . ?
Mo4 O14 2.165(4) . ?
Mo4 O13 2.235(4) . ?
Cu1 N1 1.891(16) 9 ?
Cu1 N1 1.891(16) . ?
Cu2 O4 1.979(4) . ?
Cu2 O4 1.979(4) 10 ?
Cu2 O5 2.060(6) 3_645 ?
Cu2 O11 2.065(6) 3_645 ?
Cu3 O8 1.997(5) 2_655 ?
Cu3 O8 1.997(5) . ?
Cu3 O8 1.997(5) 15 ?
Cu3 O8 1.997(5) 16_545 ?
O5 Mo4 1.971(3) 10 ?
O5 Cu2 2.060(6) 11_665 ?
O6 Mo2 2.266(4) 10 ?
O11 Mo2 1.946(3) 10 ?
O11 Cu2 2.065(6) 11_665 ?
O13 Mo4 2.235(4) 10 ?

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
O7 Mo1 O7 107.4(3) 10 . ?
O7 Mo1 O6 101.37(18) 10 . ?
O7 Mo1 O6 101.37(18) . . ?
O7 Mo1 O13 101.54(19) 10 . ?
O7 Mo1 O13 101.54(19) . . ?
O6 Mo1 O13 140.8(3) . . ?
O7 Mo1 O14 170.47(18) 10 . ?
O7 Mo1 O14 82.17(18) . . ?
O6 Mo1 O14 76.39(16) . . ?
O13 Mo1 O14 75.78(16) . . ?
O7 Mo1 O14 82.17(18) 10 10 ?
O7 Mo1 O14 170.47(18) . 10 ?
O6 Mo1 O14 76.39(16) . 10 ?
O13 Mo1 O14 75.78(16) . 10 ?
O14 Mo1 O14 88.3(2) . 10 ?
O9 Mo2 O4 105.1(2) . . ?
O9 Mo2 O11 98.5(2) . . ?
O4 Mo2 O11 98.4(2) . . ?
O9 Mo2 O10 99.0(2) . . ?
O4 Mo2 O10 94.01(19) . . ?
O11 Mo2 O10 155.1(2) . . ?
O9 Mo2 O14 95.26(19) . . ?
O4 Mo2 O14 157.74(19) . . ?
O11 Mo2 O14 87.3(2) . . ?
O10 Mo2 O14 73.63(17) . . ?
O9 Mo2 O6 166.1(2) . . ?
O4 Mo2 O6 87.8(2) . . ?
O11 Mo2 O6 74.07(18) . . ?
O10 Mo2 O6 84.89(17) . . ?
O14 Mo2 O6 72.92(18) . . ?
O9 Mo2 Mo3 88.22(16) . . ?
O4 Mo2 Mo3 128.66(15) . . ?
O11 Mo2 Mo3 128.98(17) . . ?
O10 Mo2 Mo3 34.65(13) . . ?
O14 Mo2 Mo3 41.73(11) . . ?
O6 Mo2 Mo3 87.57(12) . . ?
O1 Mo3 O8 104.8(2) . . ?
O1 Mo3 O10 99.3(2) . . ?
O8 Mo3 O10 101.7(2) . . ?
O1 Mo3 O12 98.4(2) . . ?
O8 Mo3 O12 99.8(2) . . ?
O10 Mo3 O12 147.56(19) . . ?
O1 Mo3 O14 106.1(2) . . ?
O8 Mo3 O14 149.1(2) . . ?
O10 Mo3 O14 74.73(17) . . ?
O12 Mo3 O14 74.33(18) . . ?
O1 Mo3 O7 176.6(2) . . ?
O8 Mo3 O7 78.52(19) . . ?
O10 Mo3 O7 80.50(17) . . ?
O12 Mo3 O7 80.27(17) . . ?
O14 Mo3 O7 70.56(15) . . ?
O1 Mo3 Mo2 94.62(17) . . ?
O8 Mo3 Mo2 136.38(16) . . ?
O10 Mo3 Mo2 35.79(13) . . ?
O12 Mo3 Mo2 115.78(14) . . ?
O14 Mo3 Mo2 41.76(11) . . ?
O7 Mo3 Mo2 83.26(10) . . ?
O1 Mo3 Mo4 94.60(17) . . ?
O8 Mo3 Mo4 133.39(16) . . ?
O10 Mo3 Mo4 116.64(13) . . ?
O12 Mo3 Mo4 34.70(13) . . ?
O14 Mo3 Mo4 42.12(11) . . ?
O7 Mo3 Mo4 82.53(10) . . ?
Mo2 Mo3 Mo4 81.886(19) . . ?
O3 Mo4 O2 104.9(2) . . ?
O3 Mo4 O12 101.3(2) . . ?
O2 Mo4 O12 94.5(2) . . ?
O3 Mo4 O5 94.7(2) . . ?
O2 Mo4 O5 100.7(2) . . ?
O12 Mo4 O5 154.2(2) . . ?
O3 Mo4 O14 96.1(2) . . ?
O2 Mo4 O14 157.4(2) . . ?
O12 Mo4 O14 72.94(17) . . ?
O5 Mo4 O14 85.5(2) . . ?
O3 Mo4 O13 163.9(2) . . ?
O2 Mo4 O13 88.3(2) . . ?
O12 Mo4 O13 86.50(18) . . ?
O5 Mo4 O13 73.41(19) . . ?
O14 Mo4 O13 72.51(18) . . ?
O3 Mo4 Mo3 90.92(16) . . ?
O2 Mo4 Mo3 128.74(17) . . ?
O12 Mo4 Mo3 34.22(14) . . ?
O5 Mo4 Mo3 126.61(17) . . ?
O14 Mo4 Mo3 41.16(10) . . ?
O13 Mo4 Mo3 87.71(13) . . ?
N1 Cu1 N1 180.0 9 . ?
O4 Cu2 O4 94.6(3) . 10 ?
O4 Cu2 O5 113.85(17) . 3_645 ?
O4 Cu2 O5 113.85(17) 10 3_645 ?
O4 Cu2 O11 108.68(17) . 3_645 ?
O4 Cu2 O11 108.68(17) 10 3_645 ?
O5 Cu2 O11 115.2(2) 3_645 3_645 ?
O8 Cu3 O8 130.7(3) 2_655 . ?
O8 Cu3 O8 100.01(11) 2_655 15 ?
O8 Cu3 O8 100.01(11) . 15 ?
O8 Cu3 O8 100.01(11) 2_655 16_545 ?
O8 Cu3 O8 100.01(11) . 16_545 ?
O8 Cu3 O8 130.7(3) 15 16_545 ?
Mo2 O4 Cu2 138.5(3) . . ?
Mo4 O5 Mo4 112.0(3) 10 . ?
Mo4 O5 Cu2 116.21(18) 10 11_665 ?
Mo4 O5 Cu2 116.21(18) . 11_665 ?
Mo1 O6 Mo2 110.3(2) . . ?
Mo1 O6 Mo2 110.3(2) . 10 ?
Mo2 O6 Mo2 92.3(2) . 10 ?
Mo1 O7 Mo3 106.4(2) . . ?
Mo3 O8 Cu3 149.0(3) . . ?
Mo3 O10 Mo2 109.6(2) . . ?
Mo2 O11 Mo2 114.2(3) 10 . ?
Mo2 O11 Cu2 114.63(18) 10 11_665 ?
Mo2 O11 Cu2 114.63(18) . 11_665 ?
Mo3 O12 Mo4 111.1(2) . . ?
Mo1 O13 Mo4 111.7(2) . . ?
Mo1 O13 Mo4 111.7(2) . 10 ?
Mo4 O13 Mo4 94.0(2) . 10 ?
Mo3 O14 Mo2 96.51(16) . . ?
Mo3 O14 Mo4 96.72(16) . . ?
Mo2 O14 Mo4 153.8(2) . . ?
Mo3 O14 Mo1 100.91(17) . . ?
Mo2 O14 Mo1 100.11(16) . . ?
Mo4 O14 Mo1 99.48(16) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.02
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.182

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 958 195 ' '
2 0.500 0.500 0.000 958 195 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1430701'
_audit_update_record             
;
2015-10-11 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            CMF-2
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Cu Mo7 O24'
_chemical_formula_weight         1119.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3503(4)
_cell_length_b                   10.3933(4)
_cell_length_c                   15.1733(6)
_cell_angle_alpha                76.113(4)
_cell_angle_beta                 75.040(4)
_cell_angle_gamma                62.687(4)
_cell_volume                     1387.00(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    180.00(10)
_cell_measurement_reflns_used    3813
_cell_measurement_theta_min      3.117
_cell_measurement_theta_max      29.3210

_exptl_crystal_description       black-block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1030
_exptl_absorpt_coefficient_mu    3.888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7725
_exptl_absorpt_correction_T_max  0.9263
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      180.0(10)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova (Mo) X-ray Source'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8778
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0583
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         26.37
_reflns_number_total             5559
_reflns_number_gt                4478
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0359P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   constr
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5559
_refine_ls_number_parameters     169
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0876
_refine_ls_wR_factor_gt          0.0821
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.94416(5) 0.03835(5) 0.21065(4) 0.01141(13) Uani 1 1 d . . .
Mo2 Mo 1.29692(5) -0.05971(5) 0.17300(4) 0.01087(13) Uani 1 1 d . . .
Mo3 Mo 1.09912(5) 0.47630(5) 0.25102(4) 0.01026(12) Uani 1 1 d . . .
Mo4 Mo 0.94813(5) 0.35472(5) 0.14763(4) 0.01104(13) Uani 1 1 d . . .
Mo5 Mo 1.08375(5) 0.14973(5) 0.34306(3) 0.00837(12) Uani 1 1 d . . .
Mo6 Mo 1.25786(5) 0.29164(5) 0.42392(4) 0.01222(13) Uani 1 1 d . . .
Mo7 Mo 1.44753(5) 0.06558(5) 0.27829(4) 0.01242(13) Uani 1 1 d . . .
Cu1 Cu 0.78278(8) -0.21449(8) 0.32502(5) 0.01713(18) Uani 1 1 d . . .
O1 O 1.3810(4) 0.3686(5) 0.3948(3) 0.0208(10) Uiso 1 1 d . . .
O2 O 0.9604(4) 0.0717(4) 0.3680(3) 0.0140(9) Uiso 1 1 d . . .
O3 O 1.3006(4) -0.0451(5) 0.0573(3) 0.0189(10) Uiso 1 1 d . . .
O4 O 1.0940(4) 0.1769(4) 0.4508(3) 0.0136(9) Uiso 1 1 d . . .
O5 O 1.2157(4) 0.2786(4) 0.5431(3) 0.0168(9) Uiso 1 1 d . . .
O6 O 1.4323(4) -0.2311(5) 0.2021(3) 0.0183(10) Uiso 1 1 d . . .
O7 O 1.2390(4) -0.4708(4) 0.2099(3) 0.0176(9) Uiso 1 1 d . . .
O8 O 0.7974(4) 0.5183(5) 0.1524(3) 0.0202(10) Uiso 1 1 d . . .
O9 O 1.5476(4) 0.1646(5) 0.2343(3) 0.0223(10) Uiso 1 1 d . . .
O10 O 0.8343(4) -0.0367(4) 0.2882(3) 0.0184(10) Uiso 1 1 d . . .
O11 O 1.5781(4) -0.1149(4) 0.2990(3) 0.0169(9) Uiso 1 1 d . . .
O12 O 0.9358(4) 0.0167(5) 0.1041(3) 0.0205(10) Uiso 1 1 d . . .
O13 O 1.3990(4) 0.0927(4) 0.4101(3) 0.0137(9) Uiso 1 1 d . . .
O14 O 1.4065(4) 0.0545(4) 0.1638(3) 0.0141(9) Uiso 1 1 d . . .
O15 O 0.9391(4) -0.3597(4) 0.2510(3) 0.0178(10) Uiso 1 1 d . . .
O16 O 1.1342(4) -0.1221(4) 0.2234(3) 0.0146(9) Uiso 1 1 d . . .
O17 O 1.2646(4) -0.0103(4) 0.3180(3) 0.0115(9) Uiso 1 1 d . . .
O19 O 1.0911(4) 0.4590(4) 0.3850(3) 0.0129(9) Uiso 1 1 d . . .
O20 O 0.8274(4) 0.2444(4) 0.2041(3) 0.0126(9) Uiso 1 1 d . . .
O21 O 1.2435(4) 0.2556(4) 0.2934(3) 0.0100(8) Uiso 1 1 d . . .
O22 O 1.0968(4) 0.1340(4) 0.1947(3) 0.0104(8) Uiso 1 1 d . . .
O23 O 0.9665(4) 0.3433(4) 0.2940(3) 0.0107(8) Uiso 1 1 d . . .
O24 O 0.9903(4) 0.3225(5) 0.0352(3) 0.0208(10) Uiso 1 1 d . . .
O25 O 1.1020(4) 0.4151(4) 0.1403(3) 0.0110(9) Uiso 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
Mo1 O12 1.714(4) . ?
Mo1 O10 1.723(4) . ?
Mo1 O20 1.909(4) . ?
Mo1 O16 1.928(4) . ?
Mo1 O22 2.161(4) . ?
Mo1 Mo4 3.2129(7) . ?
Mo2 O3 1.717(4) . ?
Mo2 O6 1.727(4) . ?
Mo2 O14 1.946(4) . ?
Mo2 O16 1.985(4) . ?
Mo2 O22 2.143(4) . ?
Mo2 O17 2.285(4) . ?
Mo3 O7 1.699(4) 1_565 ?
Mo3 O15 1.749(4) 1_565 ?
Mo3 O25 1.923(4) . ?
Mo3 O19 1.980(4) . ?
Mo3 O21 2.133(4) . ?
Mo3 O23 2.251(4) . ?
Mo3 Mo6 3.1906(7) . ?
Mo4 O8 1.701(4) . ?
Mo4 O24 1.723(4) . ?
Mo4 O25 1.932(4) . ?
Mo4 O20 1.975(4) . ?
Mo4 O22 2.164(4) . ?
Mo4 O23 2.247(4) . ?
Mo5 O2 1.728(4) . ?
Mo5 O4 1.761(4) . ?
Mo5 O17 1.869(4) . ?
Mo5 O23 1.893(4) . ?
Mo5 O22 2.260(4) . ?
Mo5 O21 2.267(4) . ?
Mo6 O1 1.713(5) . ?
Mo6 O5 1.735(4) . ?
Mo6 O19 1.906(4) . ?
Mo6 O13 1.932(4) . ?
Mo6 O21 2.155(4) . ?
Mo6 O4 2.393(4) . ?
Mo6 Mo7 3.2058(7) . ?
Mo7 O9 1.694(5) . ?
Mo7 O11 1.747(4) . ?
Mo7 O14 1.933(4) . ?
Mo7 O13 1.989(4) . ?
Mo7 O21 2.134(4) . ?
Mo7 O17 2.263(4) . ?
Cu1 O15 1.947(4) . ?
Cu1 O5 1.953(4) 2_756 ?
Cu1 O11 1.985(4) 1_455 ?
Cu1 O10 2.065(4) . ?
O5 Cu1 1.953(4) 2_756 ?
O7 Mo3 1.699(4) 1_545 ?
O11 Cu1 1.985(4) 1_655 ?
O15 Mo3 1.749(4) 1_545 ?

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
O12 Mo1 O10 105.6(2) . . ?
O12 Mo1 O20 98.73(18) . . ?
O10 Mo1 O20 104.32(18) . . ?
O12 Mo1 O16 97.54(18) . . ?
O10 Mo1 O16 98.80(18) . . ?
O20 Mo1 O16 146.86(17) . . ?
O12 Mo1 O22 108.90(19) . . ?
O10 Mo1 O22 145.36(17) . . ?
O20 Mo1 O22 74.06(15) . . ?
O16 Mo1 O22 73.41(16) . . ?
O12 Mo1 Mo4 95.76(15) . . ?
O10 Mo1 Mo4 137.28(14) . . ?
O20 Mo1 Mo4 34.85(12) . . ?
O16 Mo1 Mo4 114.80(13) . . ?
O22 Mo1 Mo4 42.05(9) . . ?
O3 Mo2 O6 105.4(2) . . ?
O3 Mo2 O14 97.74(19) . . ?
O6 Mo2 O14 98.35(18) . . ?
O3 Mo2 O16 99.51(19) . . ?
O6 Mo2 O16 93.64(18) . . ?
O14 Mo2 O16 155.53(17) . . ?
O3 Mo2 O22 95.55(17) . . ?
O6 Mo2 O22 156.74(18) . . ?
O14 Mo2 O22 88.46(15) . . ?
O16 Mo2 O22 72.74(15) . . ?
O3 Mo2 O17 164.12(17) . . ?
O6 Mo2 O17 89.09(17) . . ?
O14 Mo2 O17 73.36(16) . . ?
O16 Mo2 O17 85.64(15) . . ?
O22 Mo2 O17 71.50(14) . . ?
O7 Mo3 O15 104.3(2) 1_565 1_565 ?
O7 Mo3 O25 97.64(19) 1_565 . ?
O15 Mo3 O25 100.20(17) 1_565 . ?
O7 Mo3 O19 99.55(18) 1_565 . ?
O15 Mo3 O19 92.24(18) 1_565 . ?
O25 Mo3 O19 155.56(17) . . ?
O7 Mo3 O21 93.43(17) 1_565 . ?
O15 Mo3 O21 159.10(18) 1_565 . ?
O25 Mo3 O21 88.04(15) . . ?
O19 Mo3 O21 73.74(15) . . ?
O7 Mo3 O23 163.17(17) 1_565 . ?
O15 Mo3 O23 91.71(17) 1_565 . ?
O25 Mo3 O23 74.11(15) . . ?
O19 Mo3 O23 84.65(15) . . ?
O21 Mo3 O23 71.96(14) . . ?
O7 Mo3 Mo6 88.12(13) 1_565 . ?
O15 Mo3 Mo6 126.24(14) 1_565 . ?
O25 Mo3 Mo6 130.22(11) . . ?
O19 Mo3 Mo6 34.05(11) . . ?
O21 Mo3 Mo6 42.19(10) . . ?
O23 Mo3 Mo6 86.41(9) . . ?
O8 Mo4 O24 105.8(2) . . ?
O8 Mo4 O25 100.40(18) . . ?
O24 Mo4 O25 97.04(18) . . ?
O8 Mo4 O20 92.21(19) . . ?
O24 Mo4 O20 100.37(19) . . ?
O25 Mo4 O20 154.82(15) . . ?
O8 Mo4 O22 157.98(19) . . ?
O24 Mo4 O22 92.93(17) . . ?
O25 Mo4 O22 88.40(15) . . ?
O20 Mo4 O22 72.75(15) . . ?
O8 Mo4 O23 91.39(17) . . ?
O24 Mo4 O23 161.95(16) . . ?
O25 Mo4 O23 74.03(15) . . ?
O20 Mo4 O23 84.05(15) . . ?
O22 Mo4 O23 71.51(14) . . ?
O8 Mo4 Mo1 125.66(15) . . ?
O24 Mo4 Mo1 87.96(15) . . ?
O25 Mo4 Mo1 130.39(11) . . ?
O20 Mo4 Mo1 33.52(11) . . ?
O22 Mo4 Mo1 41.99(10) . . ?
O23 Mo4 Mo1 86.31(10) . . ?
O2 Mo5 O4 104.73(19) . . ?
O2 Mo5 O17 102.08(18) . . ?
O4 Mo5 O17 101.04(17) . . ?
O2 Mo5 O23 101.21(17) . . ?
O4 Mo5 O23 100.91(17) . . ?
O17 Mo5 O23 142.52(18) . . ?
O2 Mo5 O22 85.09(17) . . ?
O4 Mo5 O22 170.16(17) . . ?
O17 Mo5 O22 77.02(15) . . ?
O23 Mo5 O22 76.18(15) . . ?
O2 Mo5 O21 173.51(16) . . ?
O4 Mo5 O21 81.63(17) . . ?
O17 Mo5 O21 77.61(15) . . ?
O23 Mo5 O21 75.99(15) . . ?
O22 Mo5 O21 88.53(14) . . ?
O1 Mo6 O5 103.6(2) . . ?
O1 Mo6 O19 98.08(18) . . ?
O5 Mo6 O19 103.23(18) . . ?
O1 Mo6 O13 97.47(18) . . ?
O5 Mo6 O13 100.28(18) . . ?
O19 Mo6 O13 147.78(17) . . ?
O1 Mo6 O21 103.51(18) . . ?
O5 Mo6 O21 152.86(18) . . ?
O19 Mo6 O21 74.68(15) . . ?
O13 Mo6 O21 74.32(15) . . ?
O1 Mo6 O4 174.68(18) . . ?
O5 Mo6 O4 81.50(17) . . ?
O19 Mo6 O4 82.20(15) . . ?
O13 Mo6 O4 79.83(15) . . ?
O21 Mo6 O4 71.39(14) . . ?
O1 Mo6 Mo3 92.75(14) . . ?
O5 Mo6 Mo3 138.14(13) . . ?
O19 Mo6 Mo3 35.58(12) . . ?
O13 Mo6 Mo3 115.67(12) . . ?
O21 Mo6 Mo3 41.67(10) . . ?
O4 Mo6 Mo3 84.37(9) . . ?
O1 Mo6 Mo7 91.88(15) . . ?
O5 Mo6 Mo7 135.55(13) . . ?
O19 Mo6 Mo7 115.66(12) . . ?
O13 Mo6 Mo7 35.75(12) . . ?
O21 Mo6 Mo7 41.37(9) . . ?
O4 Mo6 Mo7 83.25(10) . . ?
Mo3 Mo6 Mo7 80.821(18) . . ?
O9 Mo7 O11 105.0(2) . . ?
O9 Mo7 O14 98.0(2) . . ?
O11 Mo7 O14 98.14(18) . . ?
O9 Mo7 O13 100.23(19) . . ?
O11 Mo7 O13 93.18(18) . . ?
O14 Mo7 O13 155.22(16) . . ?
O9 Mo7 O21 93.19(18) . . ?
O11 Mo7 O21 159.38(18) . . ?
O14 Mo7 O21 88.74(15) . . ?
O13 Mo7 O21 73.70(15) . . ?
O9 Mo7 O17 163.79(17) . . ?
O11 Mo7 O17 90.35(17) . . ?
O14 Mo7 O17 74.10(16) . . ?
O13 Mo7 O17 83.90(15) . . ?
O21 Mo7 O17 72.79(14) . . ?
O9 Mo7 Mo6 87.89(15) . . ?
O11 Mo7 Mo6 127.68(14) . . ?
O14 Mo7 Mo6 130.61(11) . . ?
O13 Mo7 Mo6 34.57(11) . . ?
O21 Mo7 Mo6 41.88(10) . . ?
O17 Mo7 Mo6 86.84(10) . . ?
O15 Cu1 O5 112.17(17) . 2_756 ?
O15 Cu1 O11 121.13(17) . 1_455 ?
O5 Cu1 O11 111.07(17) 2_756 1_455 ?
O15 Cu1 O10 104.10(18) . . ?
O5 Cu1 O10 107.93(17) 2_756 . ?
O11 Cu1 O10 98.44(17) 1_455 . ?
Mo5 O4 Mo6 107.60(19) . . ?
Mo6 O5 Cu1 164.3(2) . 2_756 ?
Mo1 O10 Cu1 144.8(2) . . ?
Mo7 O11 Cu1 136.6(2) . 1_655 ?
Mo6 O13 Mo7 109.69(18) . . ?
Mo7 O14 Mo2 116.0(2) . . ?
Mo3 O15 Cu1 145.9(2) 1_545 . ?
Mo1 O16 Mo2 111.6(2) . . ?
Mo5 O17 Mo7 109.12(18) . . ?
Mo5 O17 Mo2 109.85(16) . . ?
Mo7 O17 Mo2 92.68(15) . . ?
Mo6 O19 Mo3 110.37(19) . . ?
Mo1 O20 Mo4 111.64(18) . . ?
Mo3 O21 Mo7 152.7(2) . . ?
Mo3 O21 Mo6 96.15(15) . . ?
Mo7 O21 Mo6 96.75(14) . . ?
Mo3 O21 Mo5 101.39(14) . . ?
Mo7 O21 Mo5 100.09(15) . . ?
Mo6 O21 Mo5 99.38(16) . . ?
Mo2 O22 Mo1 97.57(16) . . ?
Mo2 O22 Mo4 151.0(2) . . ?
Mo1 O22 Mo4 95.96(14) . . ?
Mo2 O22 Mo5 101.38(14) . . ?
Mo1 O22 Mo5 100.82(16) . . ?
Mo4 O22 Mo5 101.11(15) . . ?
Mo5 O23 Mo4 110.95(17) . . ?
Mo5 O23 Mo3 110.27(16) . . ?
Mo4 O23 Mo3 92.33(15) . . ?
Mo3 O25 Mo4 114.7(2) . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.177
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.206

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 0.451 407 87 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_11
_database_code_depnum_ccdc_archive 'CCDC 1430702'
_audit_update_record             
;
2015-10-11 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            CMF-3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Cu Mo7 O24'
_chemical_formula_weight         1119.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P n m a'

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

_cell_length_a                   10.4495(7)
_cell_length_b                   19.2758(9)
_cell_length_c                   13.2417(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2667.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    180.01(13)
_cell_measurement_reflns_used    1990
_cell_measurement_theta_min      3.5280
_cell_measurement_theta_max      28.8350

_exptl_crystal_description       black-rod
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2060
_exptl_absorpt_coefficient_mu    4.043
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5298
_exptl_absorpt_correction_T_max  0.7934
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      180.01(13)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6291
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.26
_diffrn_reflns_theta_max         26.36
_reflns_number_total             2763
_reflns_number_gt                2110
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0553P)²+28.4542P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   constr
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00060(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2763
_refine_ls_number_parameters     150
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1347
_refine_ls_wR_factor_gt          0.1259
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.048
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.32510(7) 0.66397(3) 0.82662(5) 0.0171(2) Uani 1 1 d . . .
Mo2 Mo 0.80650(13) 0.7500 0.45114(8) 0.0309(3) Uani 1 2 d S . .
Mo3 Mo 0.52120(10) 0.66481(4) 0.46668(6) 0.0359(3) Uani 1 1 d . . .
Mo4 Mo 0.78048(9) 0.57495(4) 0.47489(6) 0.0336(3) Uani 1 1 d . . .
Cu1 Cu 0.54997(14) 0.7500 0.68576(11) 0.0216(4) Uani 1 2 d S . .
O1A O 0.861(3) 0.5341(7) 0.3832(16) 0.032(5) Uiso 0.62(10) 1 d P . 1
O1B O 0.900(5) 0.5302(12) 0.400(2) 0.030(9) Uiso 0.38(10) 1 d P . 2
O2 O 0.9034(6) 0.6010(3) 0.5749(5) 0.0273(14) Uani 1 1 d . . .
O3 O 0.7082(7) 0.5109(3) 0.5426(5) 0.0357(17) Uani 1 1 d . . .
O4A O 0.622(4) 0.6026(8) 0.3935(11) 0.031(5) Uiso 0.63(13) 1 d P . 1
O4B O 0.660(6) 0.5991(12) 0.3894(17) 0.023(10) Uiso 0.37(13) 1 d P . 2
O5 O 0.7044(6) 0.6676(3) 0.5440(4) 0.0229(13) Uiso 1 1 d . . .
O6A O 0.894(4) 0.6775(7) 0.3966(14) 0.020(6) Uiso 0.48(9) 1 d P A 1
O6B O 0.852(4) 0.6793(7) 0.3855(13) 0.025(6) Uiso 0.52(9) 1 d P . 2
O7 O 0.6394(11) 0.7500 0.3965(6) 0.039(3) Uani 1 2 d S . .
O8 O 0.4507(6) 0.6087(3) 0.5500(5) 0.0354(16) Uani 1 1 d . . .
O9A O 0.393(3) 0.6738(7) 0.3787(14) 0.047(5) Uiso 0.62(6) 1 d P . 1
O9B O 0.441(3) 0.6707(9) 0.3597(16) 0.021(8) Uiso 0.38(6) 1 d P . 2
O10 O 0.4818(9) 0.7500 0.5409(7) 0.032(2) Uani 1 2 d S . .
O11 O 0.7408(7) 0.7500 0.7196(6) 0.0169(16) Uani 1 2 d S . .
O12 O 0.4640(5) 0.6732(3) 0.7578(5) 0.0266(14) Uani 1 1 d . . .
O13 O 0.2348(5) 0.6062(3) 0.7583(5) 0.0229(13) Uani 1 1 d . . .
O14 O 0.8954(8) 0.7500 0.5729(6) 0.0212(18) Uani 1 2 d SU . .


_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
Mo1 O13 1.717(6) . ?
Mo1 O12 1.723(6) . ?
Mo1 O2 1.961(6) 6_557 ?
Mo1 O11 1.975(4) 6_557 ?
Mo1 O5 2.129(6) 6_557 ?
Mo1 O14 2.250(5) 6_557 ?
Mo1 Mo4 3.1733(10) 6_557 ?
Mo2 O6B 1.686(15) . ?
Mo2 O6B 1.686(15) 8_575 ?
Mo2 O6A 1.82(2) 8_575 ?
Mo2 O6A 1.82(2) . ?
Mo2 O14 1.860(9) . ?
Mo2 O7 1.890(11) . ?
Mo2 O5 2.274(6) 8_575 ?
Mo2 O5 2.274(6) . ?
Mo3 O9B 1.652(17) . ?
Mo3 O8 1.712(7) . ?
Mo3 O9A 1.783(18) . ?
Mo3 O4A 1.86(3) . ?
Mo3 O10 1.957(5) . ?
Mo3 O5 2.172(6) . ?
Mo3 O4B 2.18(6) . ?
Mo3 O7 2.255(7) . ?
Mo3 Mo4 3.2176(14) . ?
Mo4 O1A 1.673(14) . ?
Mo4 O3 1.703(6) . ?
Mo4 O4B 1.76(5) . ?
Mo4 O1B 1.81(3) . ?
Mo4 O2 1.912(6) . ?
Mo4 O4A 2.05(3) . ?
Mo4 O5 2.159(6) . ?
Mo4 O6B 2.451(14) . ?
Mo4 Mo1 3.1733(10) 6_657 ?
Cu1 O12 1.978(6) 8_575 ?
Cu1 O12 1.978(6) . ?
Cu1 O11 2.044(8) . ?
Cu1 O10 2.047(9) . ?
O2 Mo1 1.961(6) 6_657 ?
O5 Mo1 2.129(6) 6_657 ?
O7 Mo3 2.255(7) 8_575 ?
O10 Mo3 1.957(5) 8_575 ?
O11 Mo1 1.975(4) 3_566 ?
O11 Mo1 1.975(4) 6_657 ?
O14 Mo1 2.250(5) 3_566 ?
O14 Mo1 2.250(5) 6_657 ?

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
O13 Mo1 O12 104.5(3) . . ?
O13 Mo1 O2 100.2(3) . 6_557 ?
O12 Mo1 O2 93.7(3) . 6_557 ?
O13 Mo1 O11 97.9(3) . 6_557 ?
O12 Mo1 O11 97.2(3) . 6_557 ?
O2 Mo1 O11 155.8(3) 6_557 6_557 ?
O13 Mo1 O5 96.9(2) . 6_557 ?
O12 Mo1 O5 157.1(3) . 6_557 ?
O2 Mo1 O5 74.5(2) 6_557 6_557 ?
O11 Mo1 O5 87.6(3) 6_557 6_557 ?
O13 Mo1 O14 165.7(3) . 6_557 ?
O12 Mo1 O14 87.8(3) . 6_557 ?
O2 Mo1 O14 85.8(2) 6_557 6_557 ?
O11 Mo1 O14 73.1(2) 6_557 6_557 ?
O5 Mo1 O14 72.1(3) 6_557 6_557 ?
O13 Mo1 Mo4 90.3(2) . 6_557 ?
O12 Mo1 Mo4 128.1(2) . 6_557 ?
O2 Mo1 Mo4 34.48(19) 6_557 6_557 ?
O11 Mo1 Mo4 130.2(2) 6_557 6_557 ?
O5 Mo1 Mo4 42.63(15) 6_557 6_557 ?
O14 Mo1 Mo4 87.51(17) 6_557 6_557 ?
O6B Mo2 O6B 107.9(10) . 8_575 ?
O6B Mo2 O6A 105.9(8) . 8_575 ?
O6B Mo2 O6A 14.4(6) 8_575 8_575 ?
O6B Mo2 O6A 14.4(6) . . ?
O6B Mo2 O6A 105.9(8) 8_575 . ?
O6A Mo2 O6A 100.4(13) 8_575 . ?
O6B Mo2 O14 107.7(12) . . ?
O6B Mo2 O14 107.7(12) 8_575 . ?
O6A Mo2 O14 95.4(10) 8_575 . ?
O6A Mo2 O14 95.4(11) . . ?
O6B Mo2 O7 93.8(13) . . ?
O6B Mo2 O7 93.8(13) 8_575 . ?
O6A Mo2 O7 108.2(12) 8_575 . ?
O6A Mo2 O7 108.2(12) . . ?
O14 Mo2 O7 142.5(4) . . ?
O6B Mo2 O5 167.6(11) . 8_575 ?
O6B Mo2 O5 81.2(6) 8_575 8_575 ?
O6A Mo2 O5 85.1(6) 8_575 8_575 ?
O6A Mo2 O5 170.6(7) . 8_575 ?
O14 Mo2 O5 76.5(2) . 8_575 ?
O7 Mo2 O5 76.9(2) . 8_575 ?
O6B Mo2 O5 81.2(6) . . ?
O6B Mo2 O5 167.6(11) 8_575 . ?
O6A Mo2 O5 170.6(7) 8_575 . ?
O6A Mo2 O5 85.1(6) . . ?
O14 Mo2 O5 76.5(2) . . ?
O7 Mo2 O5 76.9(2) . . ?
O5 Mo2 O5 88.6(3) 8_575 . ?
O9B Mo3 O8 112.2(10) . . ?
O9B Mo3 O9A 18.3(7) . . ?
O8 Mo3 O9A 99.2(8) . . ?
O9B Mo3 O4A 83.4(13) . . ?
O8 Mo3 O4A 99.8(6) . . ?
O9A Mo3 O4A 98.4(12) . . ?
O9B Mo3 O10 105.4(9) . . ?
O8 Mo3 O10 96.7(3) . . ?
O9A Mo3 O10 95.1(7) . . ?
O4A Mo3 O10 156.7(10) . . ?
O9B Mo3 O5 148.4(12) . . ?
O8 Mo3 O5 95.2(3) . . ?
O9A Mo3 O5 165.3(9) . . ?
O4A Mo3 O5 76.4(9) . . ?
O10 Mo3 O5 85.9(3) . . ?
O9B Mo3 O4B 88.6(14) . . ?
O8 Mo3 O4B 102.8(7) . . ?
O9A Mo3 O4B 104.4(13) . . ?
O4A Mo3 O4B 7.5(8) . . ?
O10 Mo3 O4B 149.6(12) . . ?
O5 Mo3 O4B 69.5(11) . . ?
O9B Mo3 O7 82.9(9) . . ?
O8 Mo3 O7 164.0(3) . . ?
O9A Mo3 O7 94.1(7) . . ?
O4A Mo3 O7 86.9(7) . . ?
O10 Mo3 O7 73.2(3) . . ?
O5 Mo3 O7 72.1(3) . . ?
O4B Mo3 O7 82.2(9) . . ?
O9B Mo3 Mo4 119.7(11) . . ?
O8 Mo3 Mo4 90.0(2) . . ?
O9A Mo3 Mo4 134.9(8) . . ?
O4A Mo3 Mo4 36.6(8) . . ?
O10 Mo3 Mo4 127.7(3) . . ?
O5 Mo3 Mo4 41.86(15) . . ?
O4B Mo3 Mo4 31.0(9) . . ?
O7 Mo3 Mo4 86.8(2) . . ?
O1A Mo4 O3 105.3(5) . . ?
O1A Mo4 O4B 91(2) . . ?
O3 Mo4 O4B 102.3(14) . . ?
O1A Mo4 O1B 14.8(9) . . ?
O3 Mo4 O1B 104.4(7) . . ?
O4B Mo4 O1B 106(2) . . ?
O1A Mo4 O2 106.8(12) . . ?
O3 Mo4 O2 97.1(3) . . ?
O4B Mo4 O2 149.2(7) . . ?
O1B Mo4 O2 92.4(17) . . ?
O1A Mo4 O4A 98.5(15) . . ?
O3 Mo4 O4A 96.1(7) . . ?
O4B Mo4 O4A 8.7(12) . . ?
O1B Mo4 O4A 113.2(19) . . ?
O2 Mo4 O4A 147.1(5) . . ?
O1A Mo4 O5 151.8(5) . . ?
O3 Mo4 O5 102.3(3) . . ?
O4B Mo4 O5 77.8(11) . . ?
O1B Mo4 O5 151.6(8) . . ?
O2 Mo4 O5 74.7(2) . . ?
O4A Mo4 O5 73.1(6) . . ?
O1A Mo4 O6B 83.2(6) . . ?
O3 Mo4 O6B 170.1(7) . . ?
O4B Mo4 O6B 72.0(15) . . ?
O1B Mo4 O6B 85.1(9) . . ?
O2 Mo4 O6B 85.0(8) . . ?
O4A Mo4 O6B 77.4(11) . . ?
O5 Mo4 O6B 68.8(4) . . ?
O1A Mo4 Mo1 141.4(12) . 6_657 ?
O3 Mo4 Mo1 91.2(2) . 6_657 ?
O4B Mo4 Mo1 119.7(11) . 6_657 ?
O1B Mo4 Mo1 127.5(16) . 6_657 ?
O2 Mo4 Mo1 35.49(17) . 6_657 ?
O4A Mo4 Mo1 114.4(6) . 6_657 ?
O5 Mo4 Mo1 41.89(15) . 6_657 ?
O6B Mo4 Mo1 84.9(4) . 6_657 ?
O1A Mo4 Mo3 130.6(12) . . ?
O3 Mo4 Mo3 92.0(2) . . ?
O4B Mo4 Mo3 39.8(15) . . ?
O1B Mo4 Mo3 144.8(16) . . ?
O2 Mo4 Mo3 116.61(17) . . ?
O4A Mo4 Mo3 32.9(7) . . ?
O5 Mo4 Mo3 42.17(15) . . ?
O6B Mo4 Mo3 78.5(8) . . ?
Mo1 Mo4 Mo3 81.99(3) 6_657 . ?
O12 Cu1 O12 97.0(3) 8_575 . ?
O12 Cu1 O11 109.7(2) 8_575 . ?
O12 Cu1 O11 109.7(2) . . ?
O12 Cu1 O10 107.1(3) 8_575 . ?
O12 Cu1 O10 107.1(3) . . ?
O11 Cu1 O10 123.0(4) . . ?
Mo4 O2 Mo1 110.0(3) . 6_657 ?
Mo3 O4A Mo4 110.5(7) . . ?
Mo4 O4B Mo3 109.2(12) . . ?
Mo1 O5 Mo4 95.5(2) 6_657 . ?
Mo1 O5 Mo3 154.3(3) 6_657 . ?
Mo4 O5 Mo3 96.0(2) . . ?
Mo1 O5 Mo2 100.4(2) 6_657 . ?
Mo4 O5 Mo2 100.1(2) . . ?
Mo3 O5 Mo2 100.1(2) . . ?
Mo2 O6B Mo4 109.1(7) . . ?
Mo2 O7 Mo3 110.4(3) . 8_575 ?
Mo2 O7 Mo3 110.4(3) . . ?
Mo3 O7 Mo3 93.5(4) 8_575 . ?
Mo3 O10 Mo3 114.1(5) . 8_575 ?
Mo3 O10 Cu1 113.4(3) . . ?
Mo3 O10 Cu1 113.4(3) 8_575 . ?
Mo1 O11 Mo1 114.2(4) 3_566 6_657 ?
Mo1 O11 Cu1 111.5(2) 3_566 . ?
Mo1 O11 Cu1 111.5(2) 6_657 . ?
Mo1 O12 Cu1 135.7(3) . . ?
Mo2 O14 Mo1 110.5(3) . 3_566 ?
Mo2 O14 Mo1 110.5(3) . 6_657 ?
Mo1 O14 Mo1 95.0(3) 3_566 6_657 ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        26.36
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.483
_refine_diff_density_min         -1.356
_refine_diff_density_rms         0.228

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.133 -0.250 0.372 162 41 ' '
2 -0.133 0.250 0.628 162 40 ' '
3 0.367 0.250 0.872 162 42 ' '
4 0.633 -0.250 0.128 162 41 ' '
_platon_squeeze_details          
;
;
