# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018

####################################################################### 
# 
# 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_exp_17078
_database_code_depnum_ccdc_archive 'CCDC 1839453'
_audit_update_record             
;
2018-04-25 deposited with the CCDC.
2018-10-29 downloaded from the CCDC.
;
_audit_creation_date             2018-03-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C48 H80 Fe4 Mo4 N8 Na12 O76), 8(H2 O)'
_chemical_formula_sum            'C24 H56 Fe2 Mo2 N4 Na6 O46'
_chemical_formula_weight         1578.24
_chemical_melting_point          ?
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'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   10.5180(3)
_cell_length_b                   25.1402(5)
_cell_length_c                   11.0330(3)
_cell_angle_alpha                90
_cell_angle_beta                 110.479(3)
_cell_angle_gamma                90
_cell_volume                     2733.02(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4904
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.4150
_cell_measurement_theta_min      3.3390
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13230
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.985
_diffrn_reflns_theta_min         3.130
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -98.00  -5.00   1.00   17.00    --  -22.85   0.00 -30.00   93
  2  ω    -79.00  35.00   1.00   17.00    --  -22.85 -19.00-150.00  114
  3  ω     61.00 103.00   1.00   17.00    --   24.26 178.00 -60.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0312114000
_diffrn_orient_matrix_UB_12      0.0097833000
_diffrn_orient_matrix_UB_13      0.0638760000
_diffrn_orient_matrix_UB_21      -0.0638176000
_diffrn_orient_matrix_UB_22      0.0092640000
_diffrn_orient_matrix_UB_23      -0.0003277000
_diffrn_orient_matrix_UB_31      -0.0115196000
_diffrn_orient_matrix_UB_32      -0.0247811000
_diffrn_orient_matrix_UB_33      0.0251275000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6110
_reflns_number_total             6869
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.413
_refine_diff_density_min         -1.094
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         6869
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0424
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0398P)²+7.7403P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1041
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H8WA-O8W = H8WB-O8W = H5WA-O5W = H5WB-O5W
 0.85 with sigma of 0.01
 H8WA-H8WB = H5WA-H5WB
 1.388 with sigma of 0.001
3.a Free rotating group:
 O7W(H7WA,H7WB), O6W(H6WA,H6WB), O3W(H3WA,H3WB), O2W(H2WA,H2WB)
3.b Rotating group:
 O1W(H1WA,H1WB), O4W(H4WA,H4WB)
3.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C5(H5A,H5B), C3(H3A,H3B), C1(H1A,H1B), C7(H7A,H7B), C11(H11A,H11B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Mo1 Mo 0.72918(2) 0.34585(2) -0.00872(2) 0.01104(2) Uani 1 1 d . . . . .
Fe1 Fe 0.61204(2) 0.39822(2) 0.24994(2) 0.01116(4) Uani 1 1 d . . . . .
Na1 Na 0.38697(5) 0.32338(2) 0.67055(5) 0.01883(13) Uani 1 1 d . . . . .
Na2 Na 0.83513(6) 0.51846(2) 0.43366(6) 0.03336(16) Uani 1 1 d . . . . .
O10 O 0.55466(9) 0.46918(4) 0.18013(8) 0.0203(2) Uani 1 1 d . . . . .
O7 O 0.68749(9) 0.37596(3) 0.11999(8) 0.0183(2) Uani 1 1 d . . . . .
O9 O 0.79576(9) 0.28395(4) 0.04828(9) 0.0200(2) Uani 1 1 d . . . . .
O8 O 0.57360(9) 0.33479(4) -0.12558(9) 0.0184(2) Uani 1 1 d . . . . .
O14 O 0.17998(9) 0.65771(3) 0.15311(8) 0.0208(2) Uani 1 1 d . . . . .
O5 O 0.79721(9) 0.42228(3) 0.36644(8) 0.0174(2) Uani 1 1 d . . . . .
O6 O 1.00980(9) 0.39472(4) 0.46735(9) 0.0198(2) Uani 1 1 d . . . . .
O12 O 0.06950(9) 0.62020(4) -0.08384(9) 0.0220(3) Uani 1 1 d . . . . .
O13 O -0.04688(9) 0.54892(4) -0.17625(9) 0.0224(2) Uani 1 1 d . . . . .
O1 O 0.46009(9) 0.34632(4) 0.16225(9) 0.0217(3) Uani 1 1 d . . . . .
O8W O 1.02278(10) 0.51782(4) 0.36559(9) 0.0271(2) Uani 1 1 d D . . . .
O2 O 0.42834(10) 0.26329(4) 0.08660(9) 0.0232(3) Uani 1 1 d . . . . .
O1W O 0.18874(10) 0.31214(4) 0.47903(10) 0.0267(3) Uani 1 1 d . . . . .
H1WA H 0.2063 0.3228 0.4098 0.040 Uiso 1 1 d GR . . . .
H1WB H 0.1227 0.3336 0.4816 0.040 Uiso 1 1 d GR . . . .
N2 N 0.27454(9) 0.56550(4) 0.08432(9) 0.0123(2) Uani 1 1 d . . . . .
O4 O 0.51119(10) 0.37358(4) 0.56759(9) 0.0260(2) Uani 1 1 d . . . . .
N1 N 0.68871(10) 0.32476(4) 0.35731(9) 0.0127(2) Uani 1 1 d . . . . .
O15 O 0.09919(9) 0.61776(4) 0.28994(9) 0.0250(2) Uani 1 1 d . . . . .
O3 O 0.53993(10) 0.40819(4) 0.39375(9) 0.0281(2) Uani 1 1 d . . . . .
O5W O 0.24406(11) 0.39848(4) 0.70153(10) 0.0320(3) Uani 1 1 d D . . . .
O4W O 0.30374(10) 0.26896(5) 0.80388(10) 0.0316(3) Uani 1 1 d . . . . .
H4WA H 0.2162 0.2752 0.7854 0.047 Uiso 1 1 d GR . . . .
H4WB H 0.3404 0.2786 0.8858 0.047 Uiso 1 1 d GR . . . .
O11 O 0.33855(10) 0.45956(4) 0.16404(12) 0.0356(3) Uani 1 1 d . . . . .
O7W O 0.24118(13) 0.38418(5) 0.95087(11) 0.0407(4) Uani 1 1 d . . . . .
H7WA H 0.1931 0.3599 0.9714 0.061 Uiso 1 1 d G . . . .
H7WB H 0.3249 0.3748 0.9918 0.061 Uiso 1 1 d G . . . .
O6W O 0.01879(12) 0.27975(5) 0.71853(13) 0.0474(4) Uani 1 1 d . . . . .
H6WA H -0.0228 0.3098 0.7173 0.071 Uiso 1 1 d G . . . .
H6WB H -0.0458 0.2575 0.6796 0.071 Uiso 1 1 d G . . . .
O3W O 0.22306(12) 0.35843(6) 0.25540(12) 0.0474(4) Uani 1 1 d . . . . .
H3WA H 0.1674 0.3347 0.2084 0.071 Uiso 1 1 d G . . . .
H3WB H 0.1764 0.3879 0.2400 0.071 Uiso 1 1 d G . . . .
C10 C 0.05749(12) 0.57032(5) -0.10172(11) 0.0154(3) Uani 1 1 d . . . . .
C9 C 0.17845(12) 0.53604(5) -0.02735(12) 0.0164(3) Uani 1 1 d . . . . .
H9A H 0.1463 0.5037 0.0045 0.020 Uiso 1 1 calc R . . . .
H9B H 0.2262 0.5247 -0.0860 0.020 Uiso 1 1 calc R . . . .
C5 C 0.83743(12) 0.32875(5) 0.39543(12) 0.0167(3) Uani 1 1 d . . . . .
H5A H 0.8661 0.3116 0.3284 0.020 Uiso 1 1 calc R . . . .
H5B H 0.8805 0.3092 0.4775 0.020 Uiso 1 1 calc R . . . .
C6 C 0.88702(12) 0.38605(5) 0.41294(11) 0.0144(3) Uani 1 1 d . . . . .
C3 C 0.64179(13) 0.32344(5) 0.47005(11) 0.0188(3) Uani 1 1 d . . . . .
H3A H 0.7221 0.3210 0.5504 0.023 Uiso 1 1 calc R . . . .
H3B H 0.5868 0.2909 0.4643 0.023 Uiso 1 1 calc R . . . .
C2 C 0.49514(12) 0.29709(5) 0.16316(11) 0.0168(3) Uani 1 1 d . . . . .
C12 C 0.16267(12) 0.61664(5) 0.21433(12) 0.0170(3) Uani 1 1 d . . . . .
C1 C 0.62948(13) 0.28084(5) 0.26539(12) 0.0170(3) Uani 1 1 d . . . . .
H1A H 0.6147 0.2496 0.3135 0.020 Uiso 1 1 calc R . . . .
H1B H 0.6941 0.2704 0.2225 0.020 Uiso 1 1 calc R . . . .
C7 C 0.41447(12) 0.54469(5) 0.11895(12) 0.0161(3) Uani 1 1 d . . . . .
H7A H 0.4750 0.5662 0.1914 0.019 Uiso 1 1 calc R . . . .
H7B H 0.4444 0.5498 0.0441 0.019 Uiso 1 1 calc R . . . .
C8 C 0.43265(13) 0.48651(5) 0.15773(12) 0.0175(3) Uani 1 1 d . . . . .
C4 C 0.55797(12) 0.37153(5) 0.47958(12) 0.0177(3) Uani 1 1 d . . . . .
O2W O 0.10446(14) 0.20590(6) 0.52014(15) 0.0599(5) Uani 1 1 d . . . . .
H2WA H 0.1300 0.2383 0.5145 0.090 Uiso 1 1 d G . . . .
H2WB H 0.0166 0.2080 0.4980 0.090 Uiso 1 1 d G . . . .
C11 C 0.22851(13) 0.56508(5) 0.19721(12) 0.0199(3) Uani 1 1 d . . . . .
H11A H 0.3075 0.5580 0.2766 0.024 Uiso 1 1 calc R . . . .
H11B H 0.1629 0.5357 0.1866 0.024 Uiso 1 1 calc R . . . .
Na3 Na 0.65336(15) 0.52917(7) 0.50237(17) 0.1646(6) Uani 1 1 d . . . . .
H8WA H 1.0448(8) 0.54875(2) 0.34941(14) 0.029(4) Uiso 1 1 d D . . . .
H8WB H 1.0265(9) 0.49627(2) 0.30784(13) 0.062(7) Uiso 1 1 d D . . . .
H5WA H 0.24833(17) 0.39798(7) 0.78030(5) 0.046(6) Uiso 1 1 d D . . . .
H5WB H 0.16921(16) 0.38446(7) 0.65449(5) 0.088(9) Uiso 1 1 d 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 O7 1.7938(10) . ?
Mo1 O9 1.7317(9) . ?
Mo1 O8 1.7150(8) . ?
Mo1 O14 2.1270(11) 3_665 ?
Mo1 O12 2.1776(9) 3_665 ?
Mo1 N2 2.3754(10) 3_665 ?
Fe1 O10 1.9530(9) . ?
Fe1 O7 1.9480(10) . ?
Fe1 O5 2.0148(8) . ?
Fe1 O1 2.0276(9) . ?
Fe1 N1 2.1900(10) . ?
Fe1 O3 1.9995(11) . ?
Na1 O8 2.4301(9) 1_556 ?
Na1 O2 2.4651(11) 4_566 ?
Na1 O1W 2.4103(10) . ?
Na1 O4 2.3725(12) . ?
Na1 O5W 2.5102(13) . ?
Na1 O4W 2.3882(13) . ?
Na1 Na3 4.1226(19) 3_666 ?
Na2 Na2 3.3883(12) 3_766 ?
Na2 O5 2.5196(11) . ?
Na2 O6 2.7150(11) 3_766 ?
Na2 O8W 2.3780(10) 3_766 ?
Na2 O8W 2.3446(13) . ?
Na2 O5W 2.5317(12) 3_666 ?
Na2 Na3 2.3058(19) . ?
O10 C8 1.2947(16) . ?
O8 Na1 2.4301(9) 1_554 ?
O14 Mo1 2.1270(10) 3_665 ?
O14 C12 1.2813(16) . ?
O5 C6 1.2830(14) . ?
O6 Na2 2.7150(11) 3_766 ?
O6 C6 1.2381(14) . ?
O12 Mo1 2.1777(9) 3_665 ?
O12 C10 1.2688(15) . ?
O13 C10 1.2406(14) . ?
O1 C2 1.2903(16) . ?
O8W Na2 2.3781(10) 3_766 ?
O2 Na1 2.4651(11) 4_565 ?
O2 C2 1.2305(15) . ?
N2 Mo1 2.3754(10) 3_665 ?
N2 C9 1.4889(14) . ?
N2 C7 1.4807(15) . ?
N2 C11 1.4858(18) . ?
O4 C4 1.2337(18) . ?
O4 Na3 2.938(2) 3_666 ?
N1 C5 1.4743(15) . ?
N1 C3 1.4904(18) . ?
N1 C1 1.4811(15) . ?
O15 C12 1.2378(18) . ?
O3 C4 1.2869(16) . ?
O5W Na2 2.5317(12) 3_666 ?
O11 C8 1.2214(18) . ?
C10 C9 1.5179(16) . ?
C5 C6 1.5213(17) . ?
C3 C4 1.5215(19) . ?
C2 C1 1.5233(15) . ?
C12 C11 1.5122(19) . ?
C7 C8 1.5172(17) . ?
Na3 Na1 4.1225(19) 3_666 ?
Na3 O4 2.938(2) 3_666 ?
Na3 Na3 3.527(3) 3_666 ?

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 O14 155.36(4) . 3_665 ?
O7 Mo1 O12 86.00(4) . 3_665 ?
O7 Mo1 N2 84.46(4) . 3_665 ?
O9 Mo1 O7 105.76(4) . . ?
O9 Mo1 O14 90.21(4) . 3_665 ?
O9 Mo1 O12 88.77(4) . 3_665 ?
O9 Mo1 N2 157.75(4) . 3_665 ?
O8 Mo1 O7 103.32(4) . . ?
O8 Mo1 O9 106.60(4) . . ?
O8 Mo1 O14 89.46(4) . 3_665 ?
O8 Mo1 O12 158.68(4) . 3_665 ?
O8 Mo1 N2 89.65(4) . 3_665 ?
O14 Mo1 O12 75.51(4) 3_665 3_665 ?
O14 Mo1 N2 74.51(4) 3_665 3_665 ?
O12 Mo1 N2 71.98(3) 3_665 3_665 ?
O10 Fe1 O5 94.23(3) . . ?
O10 Fe1 O1 108.45(4) . . ?
O10 Fe1 N1 171.15(4) . . ?
O10 Fe1 O3 92.74(4) . . ?
O7 Fe1 O10 96.97(4) . . ?
O7 Fe1 O5 90.23(4) . . ?
O7 Fe1 O1 85.41(4) . . ?
O7 Fe1 N1 89.32(4) . . ?
O7 Fe1 O3 170.20(4) . . ?
O5 Fe1 O1 157.26(4) . . ?
O5 Fe1 N1 79.47(3) . . ?
O1 Fe1 N1 78.17(3) . . ?
O3 Fe1 O5 90.38(4) . . ?
O3 Fe1 O1 90.27(4) . . ?
O3 Fe1 N1 81.17(4) . . ?
O8 Na1 O2 105.10(3) 1_556 4_566 ?
O8 Na1 O5W 96.51(4) 1_556 . ?
O8 Na1 Na3 103.96(3) 1_556 3_666 ?
O2 Na1 O5W 155.34(4) 4_566 . ?
O2 Na1 Na3 128.61(4) 4_566 3_666 ?
O1W Na1 O8 174.99(5) . 1_556 ?
O1W Na1 O2 77.25(3) . 4_566 ?
O1W Na1 O5W 80.33(4) . . ?
O1W Na1 Na3 77.43(3) . 3_666 ?
O4 Na1 O8 88.77(4) . 1_556 ?
O4 Na1 O2 95.23(4) . 4_566 ?
O4 Na1 O1W 95.45(4) . . ?
O4 Na1 O5W 96.97(4) . . ?
O4 Na1 O4W 169.01(4) . . ?
O4 Na1 Na3 44.34(4) . 3_666 ?
O5W Na1 Na3 54.35(4) . 3_666 ?
O4W Na1 O8 81.31(4) . 1_556 ?
O4W Na1 O2 82.88(4) . 4_566 ?
O4W Na1 O1W 94.69(4) . . ?
O4W Na1 O5W 88.91(4) . . ?
O4W Na1 Na3 143.10(4) . 3_666 ?
O5 Na2 Na2 84.09(3) . 3_766 ?
O5 Na2 O6 154.27(4) . 3_766 ?
O5 Na2 O5W 129.24(4) . 3_666 ?
O6 Na2 Na2 70.51(3) 3_766 3_766 ?
O8W Na2 Na2 44.55(3) . 3_766 ?
O8W Na2 Na2 43.76(3) 3_766 3_766 ?
O8W Na2 O5 87.91(4) . . ?
O8W Na2 O5 83.64(3) 3_766 . ?
O8W Na2 O6 71.32(4) . 3_766 ?
O8W Na2 O6 80.81(3) 3_766 3_766 ?
O8W Na2 O8W 88.31(4) . 3_766 ?
O8W Na2 O5W 87.54(4) . 3_666 ?
O8W Na2 O5W 146.63(4) 3_766 3_666 ?
O5W Na2 Na2 123.81(4) 3_666 3_766 ?
O5W Na2 O6 66.51(3) 3_666 3_766 ?
Na3 Na2 Na2 136.98(5) . 3_766 ?
Na3 Na2 O5 98.33(6) . . ?
Na3 Na2 O6 102.97(5) . 3_766 ?
Na3 Na2 O8W 93.54(5) . 3_766 ?
Na3 Na2 O8W 173.65(6) . . ?
Na3 Na2 O5W 87.58(6) . 3_666 ?
C8 O10 Fe1 122.12(9) . . ?
Mo1 O7 Fe1 168.31(5) . . ?
Mo1 O8 Na1 164.64(6) . 1_554 ?
C12 O14 Mo1 123.02(9) . 3_665 ?
Fe1 O5 Na2 119.60(4) . . ?
C6 O5 Fe1 117.01(7) . . ?
C6 O5 Na2 123.03(7) . . ?
C6 O6 Na2 135.59(8) . 3_766 ?
C10 O12 Mo1 119.21(8) . 3_665 ?
C2 O1 Fe1 115.99(7) . . ?
Na2 O8W Na2 91.69(4) . 3_766 ?
C2 O2 Na1 119.08(8) . 4_565 ?
C9 N2 Mo1 104.66(7) . 3_665 ?
C7 N2 Mo1 108.35(7) . 3_665 ?
C7 N2 C9 111.31(9) . . ?
C7 N2 C11 111.55(9) . . ?
C11 N2 Mo1 109.32(7) . 3_665 ?
C11 N2 C9 111.36(10) . . ?
Na1 O4 Na3 101.30(5) . 3_666 ?
C4 O4 Na1 142.44(9) . . ?
C4 O4 Na3 100.86(9) . 3_666 ?
C5 N1 Fe1 104.48(7) . . ?
C5 N1 C3 113.05(9) . . ?
C5 N1 C1 113.34(10) . . ?
C3 N1 Fe1 107.66(7) . . ?
C1 N1 Fe1 105.74(6) . . ?
C1 N1 C3 111.85(10) . . ?
C4 O3 Fe1 119.66(9) . . ?
Na1 O5W Na2 129.00(5) . 3_666 ?
O12 C10 C9 117.26(10) . . ?
O13 C10 O12 123.27(11) . . ?
O13 C10 C9 119.47(11) . . ?
N2 C9 C10 111.27(10) . . ?
N1 C5 C6 112.53(10) . . ?
O5 C6 C5 116.73(10) . . ?
O6 C6 O5 124.48(11) . . ?
O6 C6 C5 118.77(10) . . ?
N1 C3 C4 114.15(10) . . ?
O1 C2 C1 116.85(10) . . ?
O2 C2 O1 124.34(10) . . ?
O2 C2 C1 118.81(11) . . ?
O14 C12 C11 117.98(12) . . ?
O15 C12 O14 123.13(12) . . ?
O15 C12 C11 118.83(12) . . ?
N1 C1 C2 111.46(10) . . ?
N2 C7 C8 115.41(10) . . ?
O10 C8 C7 113.39(11) . . ?
O11 C8 O10 124.84(12) . . ?
O11 C8 C7 121.76(12) . . ?
O4 C4 O3 123.53(12) . . ?
O4 C4 C3 119.20(11) . . ?
O3 C4 C3 117.26(12) . . ?
N2 C11 C12 113.36(10) . . ?
Na2 Na3 Na1 85.17(5) . 3_666 ?
Na2 Na3 O4 119.39(8) . 3_666 ?
Na2 Na3 Na3 143.68(10) . 3_666 ?
O4 Na3 Na1 34.36(3) 3_666 3_666 ?
O4 Na3 Na3 83.71(6) 3_666 3_666 ?
Na3 Na3 Na1 114.93(6) 3_666 3_666 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.125
_oxdiff_exptl_absorpt_empirical_full_min 0.917
####################################################################### 
# 
# 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_exp_17632
_database_code_depnum_ccdc_archive 'CCDC 1839456'
_audit_update_record             
;
2018-04-25 deposited with the CCDC.
2018-10-29 downloaded from the CCDC.
;
_audit_creation_date             2018-01-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H40 Fe8 Mo2 N8 O40'
_chemical_formula_sum            'C32 H40 Fe8 Mo2 N8 O40'
_chemical_formula_weight         1815.40
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
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'
N N 0.0061 0.0033 '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      tetragonal
_space_group_IT_number           121
_space_group_name_H-M_alt        'I -4 2 m'
_space_group_name_Hall           'I -4 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-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+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                   9.7754(2)
_cell_length_b                   9.7754(2)
_cell_length_c                   13.7948(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1318.21(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    2263
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.5970
_cell_measurement_theta_min      2.5480
_shelx_estimated_absorpt_T_max   0.773
_shelx_estimated_absorpt_T_min   0.613
_exptl_absorpt_coefficient_mu    2.714
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.287
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5335
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.904
_diffrn_reflns_theta_min         2.554
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -41.00  48.00   1.00   10.00    --  -22.85  57.00 120.00   89
  2  ω    -21.00   8.00   1.00   10.00    --   24.10  99.00-106.00   29
  3  ω     35.00  60.00   1.00   10.00    --   24.10  57.00-180.00   25
  4  ω    -92.00   1.00   1.00   10.00    --  -22.85 -57.00-120.00   93
  5  ω     77.00 106.00   1.00   10.00    --   24.10-178.00-150.00   29
  6  ω     78.00 104.00   1.00   10.00    --   24.10-178.00 120.00   26
  7  ω    -71.00 -42.00   1.00   10.00    --  -22.85-178.00  90.00   29
  8  ω    -96.00  -3.00   1.00   10.00    --  -22.85 -38.00 -30.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0651613000
_diffrn_orient_matrix_UB_12      -0.0256973000
_diffrn_orient_matrix_UB_13      0.0134543000
_diffrn_orient_matrix_UB_21      -0.0103397000
_diffrn_orient_matrix_UB_22      -0.0236687000
_diffrn_orient_matrix_UB_23      -0.0480160000
_diffrn_orient_matrix_UB_31      0.0302644000
_diffrn_orient_matrix_UB_32      -0.0635908000
_diffrn_orient_matrix_UB_33      0.0124758000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.675
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.861
_reflns_number_gt                938
_reflns_number_total             950
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.821
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.218
_refine_ls_abs_structure_details 
;
 Flack x determined using 340 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.20(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.335
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         950
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0600
_refine_ls_restrained_S_all      1.335
_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)+36.7463P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1384
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Mo1 Mo 0.0000 0.0000 0.5000 0.0071(5) Uani 1 8 d S T P . .
Fe1 Fe 0.19679(15) 0.19679(15) 0.68867(14) 0.0120(5) Uani 1 2 d S T P . .
O2 O 0.5102(10) 0.2764(11) 0.7484(6) 0.034(2) Uani 1 1 d . . . . .
O1 O 0.3887(8) 0.1830(11) 0.6308(6) 0.028(2) Uani 1 1 d . . . . .
N1 N 0.7496(10) 0.2504(10) 0.6597(9) 0.014(2) Uani 1 2 d S T P . .
H1 H 0.8219 0.1781 0.6621 0.017 Uiso 1 2 calc RS T P . .
O3 O 0.1051(8) 0.1051(8) 0.5742(7) 0.020(2) Uani 1 2 d S T P . .
C2 C 0.4999(13) 0.2206(10) 0.6678(7) 0.018(2) Uani 1 1 d . . . . .
C1 C 0.6308(11) 0.1913(14) 0.6113(8) 0.021(2) Uani 1 1 d . . . . .
H1A H 0.6433 0.0911 0.6053 0.026 Uiso 1 1 calc R . . . .
H1B H 0.6229 0.2299 0.5452 0.026 Uiso 1 1 calc R . . . .


_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 O3 1.776(11) 4_556 ?
Mo1 O3 1.776(11) . ?
Mo1 O3 1.776(11) 3_556 ?
Mo1 O3 1.776(11) 2 ?
Fe1 O2 2.037(10) 12_546 ?
Fe1 O2 2.037(10) 14_456 ?
Fe1 O1 2.043(9) 8 ?
Fe1 O1 2.043(9) . ?
Fe1 N1 2.216(12) 12_546 ?
Fe1 O3 2.026(11) . ?
O2 Fe1 2.037(10) 11_556 ?
O2 C2 1.243(12) . ?
O1 C2 1.256(14) . ?
N1 Fe1 2.216(12) 11_556 ?
N1 C1 1.458(13) . ?
N1 C1 1.458(13) 7_665 ?
C2 C1 1.526(15) . ?

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
O3 Mo1 O3 109.7(7) 4_556 3_556 ?
O3 Mo1 O3 109.7(7) 2 . ?
O3 Mo1 O3 109.4(3) 3_556 . ?
O3 Mo1 O3 109.4(3) 3_556 2 ?
O3 Mo1 O3 109.4(3) 4_556 2 ?
O3 Mo1 O3 109.4(3) 4_556 . ?
O2 Fe1 O2 92.8(6) 14_456 12_546 ?
O2 Fe1 O1 89.4(4) 12_546 . ?
O2 Fe1 O1 89.4(4) 14_456 8 ?
O2 Fe1 O1 175.7(4) 14_456 . ?
O2 Fe1 O1 175.7(4) 12_546 8 ?
O2 Fe1 N1 77.1(3) 14_456 12_546 ?
O2 Fe1 N1 77.1(3) 12_546 12_546 ?
O1 Fe1 O1 88.2(6) 8 . ?
O1 Fe1 N1 99.8(4) . 12_546 ?
O1 Fe1 N1 99.8(4) 8 12_546 ?
O3 Fe1 O2 89.6(3) . 12_546 ?
O3 Fe1 O2 89.6(3) . 14_456 ?
O3 Fe1 O1 94.2(3) . 8 ?
O3 Fe1 O1 94.2(3) . . ?
O3 Fe1 N1 160.5(5) . 12_546 ?
C2 O2 Fe1 120.7(9) . 11_556 ?
C2 O1 Fe1 128.1(7) . . ?
C1 N1 Fe1 109.8(6) 7_665 11_556 ?
C1 N1 Fe1 109.8(6) . 11_556 ?
C1 N1 C1 115.0(14) . 7_665 ?
Mo1 O3 Fe1 163.9(6) . . ?
O2 C2 O1 124.2(12) . . ?
O2 C2 C1 118.1(11) . . ?
O1 C2 C1 117.7(8) . . ?
N1 C1 C2 111.1(9) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.087
_oxdiff_exptl_absorpt_empirical_full_min 0.945
####################################################################### 
# 
# 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_exp_17485
_database_code_depnum_ccdc_archive 'CCDC 1839455'
_audit_update_record             
;
2018-04-25 deposited with the CCDC.
2018-10-29 downloaded from the CCDC.
;
_audit_creation_date             2017-10-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C48 H92 Cr4 Mo4 N8 Na12 O84), 4(H2 O)'
_chemical_formula_sum            'C24 H54 Cr2 Mo2 N4 Na6 O46'
_chemical_formula_weight         1568.50
_chemical_melting_point          ?
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'
Cr Cr 0.3209 0.6236 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.5265(7)
_cell_length_b                   11.0330(6)
_cell_length_c                   16.5498(10)
_cell_angle_alpha                90
_cell_angle_beta                 107.693(6)
_cell_angle_gamma                90
_cell_volume                     2700.9(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3961
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.0860
_cell_measurement_theta_min      2.7480
_shelx_estimated_absorpt_T_max   0.905
_shelx_estimated_absorpt_T_min   0.686
_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13034
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.846
_diffrn_reflns_theta_min         2.253
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00  41.00   1.00   14.00    --  -23.01 -19.00  30.00   83
  2  ω    -95.00  15.00   1.00   14.00    --  -23.01   0.00 150.00  110
  3  ω     61.00  88.00   1.00   14.00    --   24.26 178.00 150.00   27
  4  ω     65.00 104.00   1.00   14.00    --   24.26 178.00 120.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0153371000
_diffrn_orient_matrix_UB_12      -0.0108360000
_diffrn_orient_matrix_UB_13      -0.0355901000
_diffrn_orient_matrix_UB_21      0.0420630000
_diffrn_orient_matrix_UB_22      -0.0205967000
_diffrn_orient_matrix_UB_23      0.0272859000
_diffrn_orient_matrix_UB_31      -0.0172347000
_diffrn_orient_matrix_UB_32      -0.0599349000
_diffrn_orient_matrix_UB_33      -0.0029559000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5940
_reflns_number_total             6786
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.145
_refine_diff_density_min         -1.378
_refine_diff_density_rms         0.253
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6786
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0629
_refine_ls_restrained_S_all      1.144
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0706P)²+17.5632P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1725
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H3WA-O3W = H3WB-O3W = H4WA-O4W = H4WB-O4W = H1WA-O1W = H1WB-O1W
 0.85 with sigma of 0.01
 H3WA-H3WB = H4WA-H4WB = H1WA-H1WB
 1.388 with sigma of 0.001
3. Others
 Fixed Sof: Na4(0.5) O6WB(0.5) O6WA(0.5)
4.a Free rotating group:
 O7W(H7WA,H7WB), O8W(H8WA,H8WB)
4.b Rotating group:
 O5W(H5WA,H5WB), O2W(H2WA,H2WB)
4.c Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C11(H11A,H11B), C1(H1A,H1B), C7(H7A,H7B), C9(H9A,H9B), C3(H3A,H3B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Mo1 Mo 0.40107(2) 0.30269(2) 0.25323(2) 0.01560(4) Uani 1 1 d . . . . .
Cr1 Cr 0.63563(2) 0.41002(3) 0.35494(2) 0.01455(7) Uani 1 1 d . . . . .
Na3 Na 0.51422(6) 0.19492(8) 0.85769(5) 0.0254(2) Uani 1 1 d . . . . .
O10 O 0.60954(9) 0.49251(13) 0.45023(8) 0.0188(3) Uani 1 1 d . . . . .
O14 O 0.73782(9) 0.67788(14) 0.81680(9) 0.0213(4) Uani 1 1 d . . . . .
O1 O 0.67146(9) 0.24052(14) 0.39579(9) 0.0202(3) Uani 1 1 d . . . . .
O11 O 0.70600(10) 0.39300(15) 0.55810(9) 0.0266(4) Uani 1 1 d . . . . .
O3 O 0.76379(9) 0.45765(14) 0.39702(9) 0.0209(3) Uani 1 1 d . . . . .
O12 O 0.60500(10) 0.52960(15) 0.82196(9) 0.0245(4) Uani 1 1 d . . . . .
O4 O 0.89622(9) 0.43395(15) 0.37312(10) 0.0257(4) Uani 1 1 d . . . . .
O15 O 0.87358(10) 0.59850(17) 0.83473(10) 0.0290(4) Uani 1 1 d . . . . .
O5 O 0.60786(10) 0.55856(13) 0.28446(9) 0.0216(4) Uani 1 1 d . . . . .
O8 O 0.37344(10) 0.20122(14) 0.32114(9) 0.0241(4) Uani 1 1 d . . . . .
O6 O 0.58559(11) 0.62710(15) 0.15317(10) 0.0295(4) Uani 1 1 d . . . . .
O7 O 0.51252(9) 0.35137(14) 0.31123(9) 0.0211(3) Uani 1 1 d . . . . .
O13 O 0.62177(11) 0.32934(15) 0.83206(10) 0.0308(4) Uani 1 1 d . . . . .
O2 O 0.66207(12) 0.05130(15) 0.34683(10) 0.0311(4) Uani 1 1 d . . . . .
N1 N 0.66770(10) 0.34282(15) 0.25172(10) 0.0165(4) Uani 1 1 d . . . . .
N2 N 0.65731(10) 0.54131(15) 0.67894(10) 0.0161(4) Uani 1 1 d . . . . .
C8 C 0.64945(12) 0.47262(19) 0.52967(12) 0.0184(4) Uani 1 1 d . . . . .
C4 C 0.81404(12) 0.42114(19) 0.35215(12) 0.0194(5) Uani 1 1 d . . . . .
C6 C 0.60208(13) 0.5437(2) 0.20590(12) 0.0207(5) Uani 1 1 d . . . . .
C5 C 0.61405(13) 0.4157(2) 0.17788(12) 0.0205(5) Uani 1 1 d . . . . .
H5A H 0.5541 0.3777 0.1527 0.025 Uiso 1 1 calc R . . . .
H5B H 0.6455 0.4178 0.1341 0.025 Uiso 1 1 calc R . . . .
C10 C 0.61829(12) 0.4265(2) 0.79383(12) 0.0209(5) Uani 1 1 d . . . . .
C11 C 0.75736(12) 0.5515(2) 0.70710(12) 0.0228(5) Uani 1 1 d . . . . .
H11A H 0.7765 0.5991 0.6648 0.027 Uiso 1 1 calc R . . . .
H11B H 0.7840 0.4695 0.7099 0.027 Uiso 1 1 calc R . . . .
C2 C 0.66087(13) 0.16245(19) 0.33644(13) 0.0217(5) Uani 1 1 d . . . . .
C12 C 0.79289(12) 0.6114(2) 0.79267(12) 0.0204(5) Uani 1 1 d . . . . .
C1 C 0.64313(13) 0.21203(18) 0.24652(12) 0.0198(5) Uani 1 1 d . . . . .
H1A H 0.6797 0.1669 0.2169 0.024 Uiso 1 1 calc R . . . .
H1B H 0.5785 0.2019 0.2141 0.024 Uiso 1 1 calc R . . . .
C7 C 0.61961(13) 0.56123(19) 0.58645(11) 0.0192(5) Uani 1 1 d . . . . .
H7A H 0.6362 0.6441 0.5736 0.023 Uiso 1 1 calc R . . . .
H7B H 0.5529 0.5581 0.5712 0.023 Uiso 1 1 calc R . . . .
C9 C 0.62672(14) 0.42365(19) 0.70395(12) 0.0234(5) Uani 1 1 d . . . . .
H9A H 0.6703 0.3597 0.7008 0.028 Uiso 1 1 calc R . . . .
H9B H 0.5673 0.4025 0.6633 0.028 Uiso 1 1 calc R . . . .
C3 C 0.76744(12) 0.3594(2) 0.26798(12) 0.0196(5) Uani 1 1 d . . . . .
H3A H 0.7774 0.4084 0.2215 0.024 Uiso 1 1 calc R . . . .
H3B H 0.7956 0.2791 0.2672 0.024 Uiso 1 1 calc R . . . .
Na2 Na 1.0000 0.5000 0.5000 0.0215(3) Uani 1 2 d S T P . .
Na1 Na 0.76657(7) 0.20913(9) 0.54334(6) 0.0355(3) Uani 1 1 d . . . . .
O3W O 1.10466(10) 0.49139(14) 0.42052(9) 0.0273(4) Uani 1 1 d D . . . .
O4W O 0.96396(11) 0.70690(15) 0.48797(10) 0.0335(5) Uani 1 1 d D . . . .
O5W O 0.47926(11) 0.11792(17) 0.72118(10) 0.0345(5) Uani 1 1 d . . . . .
H5WA H 0.4474 0.0447 0.7140 0.052 Uiso 1 1 d GR . . . .
H5WB H 0.5300 0.0946 0.7061 0.052 Uiso 1 1 d GR . . . .
O2W O 0.89302(13) 0.12516(18) 0.50840(12) 0.0415(5) Uani 1 1 d . . . . .
H2WA H 0.9113 0.0526 0.5343 0.062 Uiso 1 1 d GR . . . .
H2WB H 0.9437 0.1713 0.5288 0.062 Uiso 1 1 d GR . . . .
Na4 Na 0.92119(16) 0.4383(2) 0.94454(14) 0.0595(7) Uani 0.5 1 d . . . . .
O1W O 0.70320(15) 0.01078(19) 0.51949(12) 0.0577(7) Uani 1 1 d D . . . .
O7W O 0.3873(3) 0.2464(3) 0.57752(18) 0.1165(17) Uani 1 1 d . . . . .
H7WA H 0.3738 0.3200 0.5827 0.175 Uiso 1 1 d G . . . .
H7WB H 0.3418 0.2017 0.5747 0.175 Uiso 1 1 d G . . . .
O9 O 0.41441(10) 0.21714(14) 0.16947(9) 0.0243(4) Uani 1 1 d . . . . .
O6WB O 1.0338(3) 0.2973(4) 1.0015(3) 0.0541(13) Uani 0.5 1 d . . . . .
O6WA O 0.9719(3) 0.4023(4) 0.9788(3) 0.0509(13) Uani 0.5 1 d . . . . .
H3WA H 1.10274(14) 0.55437(9) 0.39048(3) 0.021(6) Uiso 1 1 d D . . . .
H4WA H 0.93542(3) 0.7449(4) 0.51623(4) 0.089(14) Uiso 1 1 d D . . . .
H3WB H 1.14540(14) 0.50033(9) 0.46808(3) 0.049(9) Uiso 1 1 d D . . . .
H4WB H 0.99979(3) 0.7548(4) 0.47392(4) 0.072(12) Uiso 1 1 d D . . . .
O8W O 0.8067(2) -0.1874(4) 0.4843(2) 0.1348(12) Uani 1 1 d . . . . .
H8WA H 0.7952 -0.2331 0.5224 0.202 Uiso 1 1 d G . . . .
H8WB H 0.7908 -0.2312 0.4383 0.202 Uiso 1 1 d G . . . .
H1WA H 0.73839(4) -0.05093(9) 0.52297(4) 0.003(5) Uiso 1 1 d D . . . .
H1WB H 0.68122(4) 0.00632(9) 0.56113(4) 1.3(4) Uiso 1 1 d 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 O14 2.1261(13) 3_666 ?
Mo1 O12 2.2158(16) 3_666 ?
Mo1 O8 1.7301(16) . ?
Mo1 O7 1.7874(13) . ?
Mo1 N2 2.3796(17) 3_666 ?
Mo1 Na1 3.4690(9) 4_565 ?
Mo1 O9 1.7408(16) . ?
Cr1 O10 1.9667(15) . ?
Cr1 O1 2.0087(15) . ?
Cr1 O3 1.9694(13) . ?
Cr1 O5 1.9815(15) . ?
Cr1 O7 1.9378(13) . ?
Cr1 N1 2.0574(17) . ?
Na3 O4 2.3933(18) 4_566 ?
Na3 O6 2.4740(19) 3_666 ?
Na3 O13 2.366(2) . ?
Na3 Na2 3.2460(9) 2_646 ?
Na3 O3W 2.5280(17) 4_566 ?
Na3 O4W 2.4761(19) 2_646 ?
Na3 O5W 2.3184(19) . ?
O10 C8 1.291(2) . ?
O14 Mo1 2.1260(13) 3_666 ?
O14 C12 1.279(3) . ?
O14 Na1 2.3615(18) 2_656 ?
O1 C2 1.279(3) . ?
O1 Na1 2.4642(15) . ?
O11 C8 1.230(2) . ?
O11 Na1 2.2802(19) . ?
O3 C4 1.294(3) . ?
O12 Mo1 2.2158(16) 3_666 ?
O12 C10 1.269(3) . ?
O4 Na3 2.3933(18) 4_665 ?
O4 C4 1.225(2) . ?
O4 Na2 2.3410(14) . ?
O15 C12 1.243(2) . ?
O15 Na4 2.481(3) . ?
O5 C6 1.286(3) . ?
O8 Na4 2.484(3) 4_565 ?
O6 Na3 2.4739(19) 3_666 ?
O6 C6 1.240(3) . ?
O13 C10 1.238(3) . ?
O2 C2 1.238(3) . ?
N1 C5 1.489(2) . ?
N1 C1 1.488(3) . ?
N1 C3 1.500(2) . ?
N2 Mo1 2.3797(17) 3_666 ?
N2 C11 1.484(2) . ?
N2 C7 1.480(2) . ?
N2 C9 1.484(3) . ?
C8 C7 1.523(3) . ?
C4 C3 1.522(3) . ?
C6 C5 1.515(3) . ?
C10 C9 1.533(3) . ?
C11 C12 1.507(3) . ?
C2 C1 1.530(3) . ?
Na2 Na3 3.2461(9) 4_665 ?
Na2 Na3 3.2461(9) 2_656 ?
Na2 O4 2.3409(14) 3_766 ?
Na2 O3W 2.3831(17) 3_766 ?
Na2 O3W 2.3830(17) . ?
Na2 O4W 2.3444(16) 3_766 ?
Na2 O4W 2.3444(16) . ?
Na1 Mo1 3.4690(9) 4_666 ?
Na1 O14 2.3615(18) 2_646 ?
Na1 O2W 2.395(2) . ?
Na1 O1W 2.383(2) . ?
Na1 O9 2.7158(16) 4_666 ?
O3W Na3 2.5280(17) 4_665 ?
O4W Na3 2.4761(19) 2_656 ?
Na4 O8 2.484(3) 4_666 ?
Na4 Na4 2.913(5) 3_767 ?
Na4 O1W 2.329(4) 2_656 ?
Na4 O6WB 2.315(5) . ?
Na4 O6WA 2.486(5) 3_767 ?
Na4 O6WA 0.909(5) . ?
O1W Na4 2.329(4) 2_646 ?
O9 Na1 2.7158(16) 4_565 ?
O6WB O6WA 1.479(6) . ?
O6WA Na4 2.486(5) 3_767 ?

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
O14 Mo1 O12 75.32(6) 3_666 3_666 ?
O14 Mo1 N2 73.47(5) 3_666 3_666 ?
O14 Mo1 Na1 41.91(5) 3_666 4_565 ?
O12 Mo1 N2 72.76(6) 3_666 3_666 ?
O12 Mo1 Na1 63.84(4) 3_666 4_565 ?
O8 Mo1 O14 90.50(6) . 3_666 ?
O8 Mo1 O12 158.20(7) . 3_666 ?
O8 Mo1 O7 103.67(7) . . ?
O8 Mo1 N2 87.50(7) . 3_666 ?
O8 Mo1 Na1 115.69(5) . 4_565 ?
O8 Mo1 O9 106.23(8) . . ?
O7 Mo1 O14 156.70(6) . 3_666 ?
O7 Mo1 O12 85.39(6) . 3_666 ?
O7 Mo1 N2 88.55(6) . 3_666 ?
O7 Mo1 Na1 137.64(5) . 4_565 ?
N2 Mo1 Na1 107.45(4) 3_666 4_565 ?
O9 Mo1 O14 88.11(6) . 3_666 ?
O9 Mo1 O12 90.03(7) . 3_666 ?
O9 Mo1 O7 105.10(7) . . ?
O9 Mo1 N2 157.29(6) . 3_666 ?
O9 Mo1 Na1 50.46(5) . 4_565 ?
O10 Cr1 O1 105.33(6) . . ?
O10 Cr1 O3 91.44(6) . . ?
O10 Cr1 O5 91.62(6) . . ?
O10 Cr1 N1 173.41(7) . . ?
O1 Cr1 N1 80.32(6) . . ?
O3 Cr1 O1 89.01(6) . . ?
O3 Cr1 O5 90.18(6) . . ?
O3 Cr1 N1 85.19(6) . . ?
O5 Cr1 O1 163.04(6) . . ?
O5 Cr1 N1 82.74(7) . . ?
O7 Cr1 O10 91.93(6) . . ?
O7 Cr1 O1 87.46(6) . . ?
O7 Cr1 O3 175.66(7) . . ?
O7 Cr1 O5 92.46(6) . . ?
O7 Cr1 N1 91.72(6) . . ?
O4 Na3 O6 89.79(6) 4_566 3_666 ?
O4 Na3 Na2 46.04(4) 4_566 2_646 ?
O4 Na3 O3W 79.66(6) 4_566 4_566 ?
O4 Na3 O4W 77.92(6) 4_566 2_646 ?
O6 Na3 Na2 113.54(5) 3_666 2_646 ?
O6 Na3 O3W 158.85(7) 3_666 4_566 ?
O6 Na3 O4W 85.34(6) 3_666 2_646 ?
O13 Na3 O4 175.11(6) . 4_566 ?
O13 Na3 O6 87.14(7) . 3_666 ?
O13 Na3 Na2 138.82(5) . 2_646 ?
O13 Na3 O3W 104.44(6) . 4_566 ?
O13 Na3 O4W 105.59(6) . 2_646 ?
O3W Na3 Na2 46.73(4) 4_566 2_646 ?
O4W Na3 Na2 45.98(4) 2_646 2_646 ?
O4W Na3 O3W 74.59(6) 2_646 4_566 ?
O5W Na3 O4 85.77(7) . 4_566 ?
O5W Na3 O6 105.31(6) . 3_666 ?
O5W Na3 O13 91.38(7) . . ?
O5W Na3 Na2 114.64(6) . 2_646 ?
O5W Na3 O3W 92.24(6) . 4_566 ?
O5W Na3 O4W 160.55(7) . 2_646 ?
C8 O10 Cr1 125.88(13) . . ?
Mo1 O14 Na1 101.12(7) 3_666 2_656 ?
C12 O14 Mo1 123.45(12) . 3_666 ?
C12 O14 Na1 127.65(12) . 2_656 ?
Cr1 O1 Na1 119.06(7) . . ?
C2 O1 Cr1 114.25(12) . . ?
C2 O1 Na1 124.39(12) . . ?
C8 O11 Na1 149.79(13) . . ?
C4 O3 Cr1 115.76(12) . . ?
C10 O12 Mo1 121.74(14) . 3_666 ?
C4 O4 Na3 131.82(14) . 4_665 ?
C4 O4 Na2 131.61(15) . . ?
Na2 O4 Na3 86.57(5) . 4_665 ?
C12 O15 Na4 121.13(16) . . ?
C6 O5 Cr1 115.18(13) . . ?
Mo1 O8 Na4 149.78(10) . 4_565 ?
C6 O6 Na3 129.11(16) . 3_666 ?
Mo1 O7 Cr1 170.05(9) . . ?
C10 O13 Na3 135.32(14) . . ?
C5 N1 Cr1 105.70(12) . . ?
C5 N1 C3 111.77(16) . . ?
C1 N1 Cr1 105.96(13) . . ?
C1 N1 C5 114.00(14) . . ?
C1 N1 C3 111.18(15) . . ?
C3 N1 Cr1 107.71(11) . . ?
C11 N2 Mo1 108.03(12) . 3_666 ?
C7 N2 Mo1 107.04(12) . 3_666 ?
C7 N2 C11 111.16(16) . . ?
C7 N2 C9 111.04(14) . . ?
C9 N2 Mo1 107.52(13) . 3_666 ?
C9 N2 C11 111.82(16) . . ?
O10 C8 C7 112.18(16) . . ?
O11 C8 O10 125.25(19) . . ?
O11 C8 C7 122.57(17) . . ?
O3 C4 C3 117.57(16) . . ?
O4 C4 O3 124.03(18) . . ?
O4 C4 C3 118.41(19) . . ?
O5 C6 C5 116.79(18) . . ?
O6 C6 O5 123.6(2) . . ?
O6 C6 C5 119.63(19) . . ?
N1 C5 C6 110.03(15) . . ?
O12 C10 C9 116.47(18) . . ?
O13 C10 O12 125.1(2) . . ?
O13 C10 C9 118.36(19) . . ?
N2 C11 C12 112.18(17) . . ?
O1 C2 C1 116.70(18) . . ?
O2 C2 O1 124.6(2) . . ?
O2 C2 C1 118.69(18) . . ?
O14 C12 C11 117.14(15) . . ?
O15 C12 O14 123.13(19) . . ?
O15 C12 C11 119.7(2) . . ?
N1 C1 C2 108.85(15) . . ?
N2 C7 C8 116.37(16) . . ?
N2 C9 C10 112.44(16) . . ?
N1 C3 C4 113.36(17) . . ?
Na3 Na2 Na3 180.0 2_656 4_665 ?
O4 Na2 Na3 47.39(4) . 4_665 ?
O4 Na2 Na3 132.61(4) 3_766 4_665 ?
O4 Na2 Na3 132.61(4) . 2_656 ?
O4 Na2 Na3 47.39(4) 3_766 2_656 ?
O4 Na2 O4 180.0 3_766 . ?
O4 Na2 O3W 83.77(5) 3_766 3_766 ?
O4 Na2 O3W 83.77(5) . . ?
O4 Na2 O3W 96.23(5) 3_766 . ?
O4 Na2 O3W 96.24(5) . 3_766 ?
O4 Na2 O4W 81.64(5) 3_766 . ?
O4 Na2 O4W 81.64(5) . 3_766 ?
O4 Na2 O4W 98.37(5) . . ?
O4 Na2 O4W 98.36(5) 3_766 3_766 ?
O3W Na2 Na3 50.58(4) . 4_665 ?
O3W Na2 Na3 129.42(4) . 2_656 ?
O3W Na2 Na3 129.42(4) 3_766 4_665 ?
O3W Na2 Na3 50.58(4) 3_766 2_656 ?
O3W Na2 O3W 180.0 . 3_766 ?
O4W Na2 Na3 130.59(4) 3_766 2_656 ?
O4W Na2 Na3 49.41(4) . 2_656 ?
O4W Na2 Na3 49.41(4) 3_766 4_665 ?
O4W Na2 Na3 130.59(4) . 4_665 ?
O4W Na2 O3W 79.80(6) . 3_766 ?
O4W Na2 O3W 79.80(6) 3_766 . ?
O4W Na2 O3W 100.20(6) 3_766 3_766 ?
O4W Na2 O3W 100.20(6) . . ?
O4W Na2 O4W 180.0 . 3_766 ?
O14 Na1 Mo1 36.97(4) 2_646 4_666 ?
O14 Na1 O1 143.58(7) 2_646 . ?
O14 Na1 O2W 116.75(7) 2_646 . ?
O14 Na1 O1W 83.96(7) 2_646 . ?
O14 Na1 O9 63.89(5) 2_646 4_666 ?
O1 Na1 Mo1 174.07(5) . 4_666 ?
O1 Na1 O9 146.26(7) . 4_666 ?
O11 Na1 Mo1 93.93(5) . 4_666 ?
O11 Na1 O14 83.64(7) . 2_646 ?
O11 Na1 O1 80.71(6) . . ?
O11 Na1 O2W 139.91(8) . . ?
O11 Na1 O1W 132.21(9) . . ?
O11 Na1 O9 86.04(6) . 4_666 ?
O2W Na1 Mo1 86.51(5) . 4_666 ?
O2W Na1 O1 95.94(7) . . ?
O2W Na1 O9 74.81(6) . 4_666 ?
O1W Na1 Mo1 102.94(5) . 4_666 ?
O1W Na1 O1 82.65(6) . . ?
O1W Na1 O2W 86.12(8) . . ?
O1W Na1 O9 127.77(7) . 4_666 ?
O9 Na1 Mo1 29.62(4) 4_666 4_666 ?
Na2 O3W Na3 82.69(5) . 4_665 ?
Na2 O4W Na3 84.61(6) . 2_656 ?
O15 Na4 O8 83.75(8) . 4_666 ?
O15 Na4 Na4 97.74(14) . 3_767 ?
O15 Na4 O6WA 82.76(13) . 3_767 ?
O8 Na4 Na4 142.34(16) 4_666 3_767 ?
O8 Na4 O6WA 147.60(17) 4_666 3_767 ?
O1W Na4 O15 81.77(10) 2_656 . ?
O1W Na4 O8 111.08(11) 2_656 4_666 ?
O1W Na4 Na4 106.35(14) 2_656 3_767 ?
O1W Na4 O6WA 95.94(16) 2_656 3_767 ?
O6WB Na4 O15 142.81(18) . . ?
O6WB Na4 O8 85.31(14) . 4_666 ?
O6WB Na4 Na4 70.84(14) . 3_767 ?
O6WB Na4 O1W 135.14(18) . 2_656 ?
O6WB Na4 O6WA 87.87(17) . 3_767 ?
O6WA Na4 O15 140.9(4) . . ?
O6WA Na4 O8 103.1(3) . 4_666 ?
O6WA Na4 Na4 53.8(3) . 3_767 ?
O6WA Na4 Na4 17.15(11) 3_767 3_767 ?
O6WA Na4 O1W 128.2(4) . 2_656 ?
O6WA Na4 O6WB 18.2(3) . . ?
O6WA Na4 O6WA 70.9(4) . 3_767 ?
Na4 O1W Na1 127.30(12) 2_646 . ?
Mo1 O9 Na1 99.92(7) . 4_565 ?
O6WA O6WB Na4 11.05(17) . . ?
Na4 O6WA Na4 109.1(4) . 3_767 ?
Na4 O6WA O6WB 150.8(5) . . ?
O6WB O6WA Na4 98.2(3) . 3_767 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.134
_oxdiff_exptl_absorpt_empirical_full_min 0.888
####################################################################### 
# 
# 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_exp_17400
_database_code_depnum_ccdc_archive 'CCDC 1839454'
_audit_update_record             
;
2018-04-25 deposited with the CCDC.
2018-10-29 downloaded from the CCDC.
;
_audit_creation_date             2017-10-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C48 H96 Al4 Mo4 N8 Na12 O84), 4(H2 O)'
_chemical_formula_sum            'C24 H56 Al2 Mo2 N4 Na6 O46'
_chemical_formula_weight         1520.48
_chemical_melting_point          ?
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'
Al Al 0.0645 0.0514 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.4271(4)
_cell_length_b                   11.0633(2)
_cell_length_c                   16.3607(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.399(2)
_cell_angle_gamma                90
_cell_volume                     2664.59(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3958
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.4680
_cell_measurement_theta_min      2.4430
_shelx_estimated_absorpt_T_max   0.876
_shelx_estimated_absorpt_T_min   0.773
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12903
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.878
_diffrn_reflns_theta_min         2.256
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      9.00  47.00   1.00    4.50    --   24.26 -99.00-120.00   38
  2  ω    -46.00  37.00   1.00    4.50    --  -22.85  57.00-180.00   83
  3  ω    -93.00 -65.00   1.00    4.50    --  -22.85 -57.00 -90.00   28
  4  ω    -94.00  10.00   1.00    4.50    --  -22.85 -77.00  30.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0172195000
_diffrn_orient_matrix_UB_12      0.0204609000
_diffrn_orient_matrix_UB_13      -0.0332261000
_diffrn_orient_matrix_UB_21      0.0017784000
_diffrn_orient_matrix_UB_22      0.0598637000
_diffrn_orient_matrix_UB_23      0.0159080000
_diffrn_orient_matrix_UB_31      0.0449730000
_diffrn_orient_matrix_UB_32      -0.0102754000
_diffrn_orient_matrix_UB_33      0.0265589000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5769
_reflns_number_total             6712
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.333
_refine_diff_density_min         -2.255
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         6712
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0513
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.089
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0575P)²+11.3175P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1350
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H2WA-O2W = H2WB-O2W = H1WA-O1W = H1WB-O1W
 0.85 with sigma of 0.01
 H2WA-H2WB = H1WA-H1WB
 1.388 with sigma of 0.001
 H6WB-H7WB
 1.8 with sigma of 0.01
3. Others
 Fixed Sof: Na4(0.5)
4.a Free rotating group:
 O8W(H8WA,H8WB), O3W(H3WA,H3WB), O7W(H7WA,H7WB)
4.b Rotating group:
 O6W(H6WA,H6WB), O5W(H5WA,H5WB), O4W(H4WA,H4WB)
4.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C11(H11A,H11B), C9(H9A,H9B), C1(H1A,H1B), C5(H5A,H5B), C3(H3A,H3B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Mo1 Mo 0.59666(2) 0.69364(2) 0.74617(2) 0.01376(3) Uani 1 1 d . . . . .
Al1 Al 0.36570(3) 0.59063(4) 0.64424(2) 0.01315(9) Uani 1 1 d . . . . .
Na1 Na 0.0000 0.5000 0.5000 0.0192(2) Uani 1 2 d S T P . .
Na3 Na 0.48886(4) 0.80624(6) 0.14312(4) 0.02302(16) Uani 1 1 d . . . . .
Na2 Na 0.23517(5) 0.79279(6) 0.45821(4) 0.03001(18) Uani 1 1 d . . . . .
O10 O 0.38971(6) 0.51801(10) 0.55251(6) 0.0172(2) Uani 1 1 d . . . . .
O3 O 0.24159(7) 0.54794(10) 0.60279(6) 0.0184(3) Uani 1 1 d . . . . .
O14 O 0.26342(7) 0.32309(10) 0.18412(6) 0.0191(3) Uani 1 1 d . . . . .
O12 O 0.39399(7) 0.47249(10) 0.17687(6) 0.0212(3) Uani 1 1 d . . . . .
O1 O 0.39109(7) 0.44789(10) 0.71150(6) 0.0187(3) Uani 1 1 d . . . . .
O15 O 0.12694(7) 0.40110(11) 0.16626(7) 0.0244(3) Uani 1 1 d . . . . .
O5 O 0.33385(7) 0.75383(10) 0.60682(6) 0.0181(3) Uani 1 1 d . . . . .
O7 O 0.48467(6) 0.64363(10) 0.68932(6) 0.0174(2) Uani 1 1 d . . . . .
O4 O 0.10665(7) 0.56635(11) 0.62446(7) 0.0229(3) Uani 1 1 d . . . . .
O11 O 0.29194(7) 0.60916(10) 0.44064(6) 0.0221(3) Uani 1 1 d . . . . .
O1W O -0.10417(7) 0.50797(10) 0.58053(7) 0.0256(3) Uani 1 1 d D . . . .
O2 O 0.41309(8) 0.37054(11) 0.84193(7) 0.0260(3) Uani 1 1 d . . . . .
O8 O 0.62240(7) 0.79461(10) 0.67716(7) 0.0217(3) Uani 1 1 d . . . . .
O13 O 0.37949(8) 0.67311(11) 0.16852(7) 0.0279(3) Uani 1 1 d . . . . .
O9 O 0.58459(7) 0.77946(10) 0.83061(7) 0.0229(3) Uani 1 1 d . . . . .
O6 O 0.34403(9) 0.94265(10) 0.65456(7) 0.0281(3) Uani 1 1 d . . . . .
O2W O 0.03371(8) 0.29291(11) 0.51246(8) 0.0297(3) Uani 1 1 d D . . . .
O6W O 0.52162(8) 0.88481(12) 0.27972(8) 0.0348(3) Uani 1 1 d . . . . .
H6WA H 0.5347 0.9638 0.2805 0.052 Uiso 1 1 d GR . . . .
H6WB H 0.5731 0.8538 0.3150 0.052 Uiso 1 1 d DGR . . . .
N1 N 0.33340(8) 0.65620(11) 0.75067(7) 0.0151(3) Uani 1 1 d . . . . .
O5W O 0.11021(9) 0.87468(12) 0.49592(8) 0.0354(3) Uani 1 1 d . . . . .
H5WA H 0.0946 0.9474 0.4724 0.053 Uiso 1 1 d GR . . . .
H5WB H 0.1249 0.8906 0.5519 0.053 Uiso 1 1 d GR . . . .
N2 N 0.34382(7) 0.46082(11) 0.32257(7) 0.0129(3) Uani 1 1 d . . . . .
C10 C 0.38207(9) 0.57593(14) 0.20621(9) 0.0185(3) Uani 1 1 d . . . . .
C8 C 0.34956(9) 0.53300(13) 0.47182(8) 0.0151(3) Uani 1 1 d . . . . .
C12 C 0.20790(9) 0.38923(14) 0.20819(8) 0.0172(3) Uani 1 1 d . . . . .
C7 C 0.38091(9) 0.44242(14) 0.41615(8) 0.0170(3) Uani 1 1 d . . . . .
H7A H 0.4480 0.4456 0.4319 0.020 Uiso 1 1 calc R . . . .
H7B H 0.3640 0.3603 0.4299 0.020 Uiso 1 1 calc R . . . .
C6 C 0.34384(10) 0.83287(14) 0.66625(9) 0.0187(3) Uani 1 1 d . . . . .
C2 C 0.39760(9) 0.45565(14) 0.79169(9) 0.0175(3) Uani 1 1 d . . . . .
C4 C 0.18943(9) 0.57996(13) 0.64674(9) 0.0170(3) Uani 1 1 d . . . . .
C11 C 0.24338(9) 0.45149(15) 0.29371(9) 0.0206(4) Uani 1 1 d . . . . .
H11A H 0.2170 0.5337 0.2895 0.025 Uiso 1 1 calc R . . . .
H11B H 0.2234 0.4060 0.3370 0.025 Uiso 1 1 calc R . . . .
C9 C 0.37497(11) 0.57837(14) 0.29720(9) 0.0228(4) Uani 1 1 d . . . . .
H9A H 0.4351 0.5985 0.3375 0.027 Uiso 1 1 calc R . . . .
H9B H 0.3319 0.6426 0.3015 0.027 Uiso 1 1 calc R . . . .
C1 C 0.38647(10) 0.58217(14) 0.82320(8) 0.0183(3) Uani 1 1 d . . . . .
H1A H 0.3549 0.5782 0.8676 0.022 Uiso 1 1 calc R . . . .
H1B H 0.4469 0.6192 0.8490 0.022 Uiso 1 1 calc R . . . .
C5 C 0.35766(10) 0.78536(13) 0.75603(9) 0.0183(3) Uani 1 1 d . . . . .
H5A H 0.4218 0.7959 0.7907 0.022 Uiso 1 1 calc R . . . .
H5B H 0.3189 0.8307 0.7839 0.022 Uiso 1 1 calc R . . . .
C3 C 0.23356(9) 0.63820(14) 0.73315(9) 0.0175(3) Uani 1 1 d . . . . .
H3A H 0.2045 0.7175 0.7352 0.021 Uiso 1 1 calc R . . . .
H3B H 0.2229 0.5866 0.7786 0.021 Uiso 1 1 calc R . . . .
O4W O 0.30234(11) 0.98773(14) 0.48367(9) 0.0461(4) Uani 1 1 d . . . . .
H4WA H 0.3370 0.9987 0.5402 0.069 Uiso 1 1 d GR . . . .
H4WB H 0.2600 1.0495 0.4775 0.069 Uiso 1 1 d GR . . . .
O8W O 0.06445(11) 0.55861(15) 0.05211(10) 0.0748(5) Uani 1 1 d . . . . .
H8WA H 0.0231 0.6014 0.0186 0.112 Uiso 1 1 d G . . . .
H8WB H 0.1126 0.5631 0.0372 0.112 Uiso 1 1 d G . . . .
O3W O 0.18896(13) 0.1798(2) 0.51098(12) 0.1070(7) Uani 1 1 d . . . . .
H3WA H 0.1970 0.2410 0.4826 0.161 Uiso 1 1 d G . . . .
H3WB H 0.2383 0.1629 0.5493 0.161 Uiso 1 1 d G . . . .
O7W O 0.6268(3) 0.75007(17) 0.41562(13) 0.1260(14) Uani 1 1 d . . . . .
H7WA H 0.6717 0.7273 0.3994 0.189 Uiso 1 1 d G . . . .
H7WB H 0.5808 0.7198 0.3789 0.189 Uiso 1 1 d DG . . . .
Na4 Na -0.0291(2) 0.6997(3) -0.00429(19) 0.0972(11) Uani 0.5 1 d . . . . .
H2WA H 0.08361(3) 0.2550(5) 0.52286(9) 0.030(5) Uiso 1 1 d D . . . .
H1WA H -0.09937(9) 0.44794(9) 0.61408(4) 0.041(6) Uiso 1 1 d D . . . .
H2WB H -0.00662(3) 0.2470(4) 0.52143(9) 0.058(7) Uiso 1 1 d D . . . .
H1WB H -0.15157(9) 0.49991(10) 0.53808(4) 0.055(7) Uiso 1 1 d 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 Na2 3.4913(6) 4_676 ?
Mo1 O14 2.1266(9) 3_666 ?
Mo1 O12 2.2081(11) 3_666 ?
Mo1 O7 1.7874(9) . ?
Mo1 O8 1.7172(12) . ?
Mo1 O9 1.7316(12) . ?
Mo1 N2 2.3762(12) 3_666 ?
Al1 O10 1.8350(11) . ?
Al1 O3 1.8902(10) . ?
Al1 O1 1.8975(11) . ?
Al1 O5 1.9226(11) . ?
Al1 O7 1.8565(10) . ?
Al1 N1 2.0799(13) . ?
Na1 Na3 3.2168(7) 2_545 ?
Na1 Na3 3.2168(7) 4_576 ?
Na1 O4 2.3213(10) 3_566 ?
Na1 O4 2.3213(10) . ?
Na1 O1W 2.3648(13) . ?
Na1 O1W 2.3648(13) 3_566 ?
Na1 O2W 2.3447(12) 3_566 ?
Na1 O2W 2.3447(12) . ?
Na3 Na1 3.2168(6) 2 ?
Na3 O4 2.3904(13) 4_675 ?
Na3 O1W 2.5405(13) 4_675 ?
Na3 O2 2.4397(14) 3_666 ?
Na3 O13 2.3682(14) . ?
Na3 O2W 2.4682(14) 2 ?
Na3 O6W 2.3087(14) . ?
Na2 Mo1 3.4914(6) 4_575 ?
Na2 O14 2.3591(13) 2 ?
Na2 O5 2.4903(11) . ?
Na2 O11 2.2645(13) . ?
Na2 O9 2.7374(12) 4_575 ?
Na2 O5W 2.3725(17) . ?
Na2 O4W 2.3749(17) . ?
Na2 Na4 3.504(4) 4_676 ?
O10 C8 1.2903(15) . ?
O3 C4 1.2791(19) . ?
O14 Mo1 2.1266(9) 3_666 ?
O14 Na2 2.3590(13) 2_545 ?
O14 C12 1.2752(19) . ?
O12 Mo1 2.2081(11) 3_666 ?
O12 C10 1.2754(19) . ?
O1 C2 1.2884(18) . ?
O15 C12 1.2391(16) . ?
O15 Na4 2.855(3) 3_565 ?
O5 C6 1.2822(18) . ?
O4 Na3 2.3903(13) 4_576 ?
O4 C4 1.2280(17) . ?
O11 C8 1.2203(17) . ?
O1W Na3 2.5405(13) 4_576 ?
O2 Na3 2.4397(14) 3_666 ?
O2 C2 1.2254(18) . ?
O13 C10 1.2340(19) . ?
O9 Na2 2.7373(12) 4_676 ?
O6 C6 1.2296(19) . ?
O2W Na3 2.4682(14) 2_545 ?
N1 C1 1.4724(17) . ?
N1 C5 1.4730(19) . ?
N1 C3 1.4934(18) . ?
N2 Mo1 2.3762(12) 3_666 ?
N2 C7 1.4795(16) . ?
N2 C11 1.4823(17) . ?
N2 C9 1.488(2) . ?
C10 C9 1.525(2) . ?
C8 C7 1.527(2) . ?
C12 C11 1.5078(19) . ?
C6 C5 1.514(2) . ?
C2 C1 1.519(2) . ?
C4 C3 1.5172(19) . ?
O8W Na4 2.138(3) . ?
O8W Na4 2.970(3) 3_565 ?
Na4 Na2 3.504(4) 4_575 ?
Na4 O15 2.855(3) 3_565 ?
Na4 O8W 2.970(3) 3_565 ?

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
O14 Mo1 Na2 41.35(3) 3_666 4_676 ?
O14 Mo1 O12 74.87(4) 3_666 3_666 ?
O14 Mo1 N2 73.58(4) 3_666 3_666 ?
O12 Mo1 Na2 63.45(3) 3_666 4_676 ?
O12 Mo1 N2 72.70(4) 3_666 3_666 ?
O7 Mo1 Na2 137.69(4) . 4_676 ?
O7 Mo1 O14 156.97(5) . 3_666 ?
O7 Mo1 O12 85.83(4) . 3_666 ?
O7 Mo1 N2 88.93(4) . 3_666 ?
O8 Mo1 Na2 115.61(4) . 4_676 ?
O8 Mo1 O14 90.69(5) . 3_666 ?
O8 Mo1 O12 158.11(5) . 3_666 ?
O8 Mo1 O7 103.70(5) . . ?
O8 Mo1 O9 105.61(5) . . ?
O8 Mo1 N2 87.62(5) . 3_666 ?
O9 Mo1 Na2 50.48(4) . 4_676 ?
O9 Mo1 O14 87.36(5) . 3_666 ?
O9 Mo1 O12 90.33(5) . 3_666 ?
O9 Mo1 O7 105.49(5) . . ?
O9 Mo1 N2 157.06(4) . 3_666 ?
N2 Mo1 Na2 107.03(3) 3_666 4_676 ?
O10 Al1 O3 91.59(5) . . ?
O10 Al1 O1 93.03(5) . . ?
O10 Al1 O5 104.22(5) . . ?
O10 Al1 O7 92.63(5) . . ?
O10 Al1 N1 174.22(6) . . ?
O3 Al1 O1 90.65(5) . . ?
O3 Al1 O5 89.16(5) . . ?
O3 Al1 N1 85.24(5) . . ?
O1 Al1 O5 162.75(5) . . ?
O1 Al1 N1 82.20(5) . . ?
O5 Al1 N1 80.59(5) . . ?
O7 Al1 O3 175.21(5) . . ?
O7 Al1 O1 91.40(5) . . ?
O7 Al1 O5 87.60(5) . . ?
O7 Al1 N1 90.75(5) . . ?
Na3 Na1 Na3 180.0 2_545 4_576 ?
O4 Na1 Na3 132.15(3) 3_566 4_576 ?
O4 Na1 Na3 47.85(3) 3_566 2_545 ?
O4 Na1 Na3 132.15(3) . 2_545 ?
O4 Na1 Na3 47.85(3) . 4_576 ?
O4 Na1 O4 180.0 3_566 . ?
O4 Na1 O1W 94.53(4) 3_566 . ?
O4 Na1 O1W 85.47(4) 3_566 3_566 ?
O4 Na1 O1W 94.53(4) . 3_566 ?
O4 Na1 O1W 85.47(4) . . ?
O4 Na1 O2W 81.25(4) . 3_566 ?
O4 Na1 O2W 81.25(4) 3_566 . ?
O4 Na1 O2W 98.75(4) . . ?
O4 Na1 O2W 98.75(4) 3_566 3_566 ?
O1W Na1 Na3 51.43(3) 3_566 2_545 ?
O1W Na1 Na3 128.57(3) . 2_545 ?
O1W Na1 Na3 51.43(3) . 4_576 ?
O1W Na1 Na3 128.57(3) 3_566 4_576 ?
O1W Na1 O1W 180.0 . 3_566 ?
O2W Na1 Na3 130.28(3) . 4_576 ?
O2W Na1 Na3 49.72(3) 3_566 4_576 ?
O2W Na1 Na3 49.72(3) . 2_545 ?
O2W Na1 Na3 130.28(3) 3_566 2_545 ?
O2W Na1 O1W 80.91(4) 3_566 . ?
O2W Na1 O1W 80.91(4) . 3_566 ?
O2W Na1 O1W 99.09(4) . . ?
O2W Na1 O1W 99.09(4) 3_566 3_566 ?
O2W Na1 O2W 180.0 . 3_566 ?
O4 Na3 Na1 46.05(3) 4_675 2 ?
O4 Na3 O1W 80.26(4) 4_675 4_675 ?
O4 Na3 O2 90.76(5) 4_675 3_666 ?
O4 Na3 O2W 77.39(4) 4_675 2 ?
O1W Na3 Na1 46.70(3) 4_675 2 ?
O2 Na3 Na1 116.15(4) 3_666 2 ?
O2 Na3 O1W 161.37(5) 3_666 4_675 ?
O2 Na3 O2W 86.99(4) 3_666 2 ?
O13 Na3 Na1 137.58(3) . 2 ?
O13 Na3 O4 176.27(5) . 4_675 ?
O13 Na3 O1W 103.16(5) . 4_675 ?
O13 Na3 O2 86.37(5) . 3_666 ?
O13 Na3 O2W 104.81(5) . 2 ?
O2W Na3 Na1 46.44(3) 2 2 ?
O2W Na3 O1W 75.18(4) 2 4_675 ?
O6W Na3 Na1 114.20(4) . 2 ?
O6W Na3 O4 86.96(5) . 4_675 ?
O6W Na3 O1W 91.11(5) . 4_675 ?
O6W Na3 O2 104.78(5) . 3_666 ?
O6W Na3 O13 91.46(5) . . ?
O6W Na3 O2W 160.62(5) . 2 ?
Mo1 Na2 Na4 117.90(6) 4_575 4_676 ?
O14 Na2 Mo1 36.55(3) 2 4_575 ?
O14 Na2 O5 143.60(5) 2 . ?
O14 Na2 O9 62.93(4) 2 4_575 ?
O14 Na2 O5W 116.77(5) 2 . ?
O14 Na2 O4W 84.94(5) 2 . ?
O14 Na2 Na4 81.61(6) 2 4_676 ?
O5 Na2 Mo1 172.48(4) . 4_575 ?
O5 Na2 O9 145.65(5) . 4_575 ?
O5 Na2 Na4 62.20(6) . 4_676 ?
O11 Na2 Mo1 93.29(3) . 4_575 ?
O11 Na2 O14 83.34(5) . 2 ?
O11 Na2 O5 79.74(4) . . ?
O11 Na2 O9 85.03(4) . 4_575 ?
O11 Na2 O5W 138.66(6) . . ?
O11 Na2 O4W 132.22(6) . . ?
O11 Na2 Na4 67.85(6) . 4_676 ?
O9 Na2 Mo1 29.21(3) 4_575 4_575 ?
O9 Na2 Na4 137.76(6) 4_575 4_676 ?
O5W Na2 Mo1 86.47(3) . 4_575 ?
O5W Na2 O5 96.85(5) . . ?
O5W Na2 O9 74.90(4) . 4_575 ?
O5W Na2 O4W 87.33(6) . . ?
O5W Na2 Na4 145.79(6) . 4_676 ?
O4W Na2 Mo1 103.92(4) . 4_575 ?
O4W Na2 O5 83.03(5) . . ?
O4W Na2 O9 128.70(5) . 4_575 ?
O4W Na2 Na4 64.66(7) . 4_676 ?
C8 O10 Al1 128.90(10) . . ?
C4 O3 Al1 117.98(9) . . ?
Mo1 O14 Na2 102.09(5) 3_666 2_545 ?
C12 O14 Mo1 123.51(8) . 3_666 ?
C12 O14 Na2 126.28(8) . 2_545 ?
C10 O12 Mo1 121.63(10) . 3_666 ?
C2 O1 Al1 118.35(10) . . ?
C12 O15 Na4 129.65(12) . 3_565 ?
Al1 O5 Na2 119.79(5) . . ?
C6 O5 Al1 115.96(9) . . ?
C6 O5 Na2 121.47(9) . . ?
Mo1 O7 Al1 172.46(7) . . ?
Na1 O4 Na3 86.10(3) . 4_576 ?
C4 O4 Na1 134.47(10) . . ?
C4 O4 Na3 130.74(10) . 4_576 ?
C8 O11 Na2 145.83(9) . . ?
Na1 O1W Na3 81.87(4) . 4_576 ?
C2 O2 Na3 132.37(11) . 3_666 ?
C10 O13 Na3 135.34(10) . . ?
Mo1 O9 Na2 100.32(5) . 4_676 ?
Na1 O2W Na3 83.84(4) . 2_545 ?
C1 N1 Al1 105.43(9) . . ?
C1 N1 C5 114.93(10) . . ?
C1 N1 C3 111.93(12) . . ?
C5 N1 Al1 105.54(9) . . ?
C5 N1 C3 111.71(12) . . ?
C3 N1 Al1 106.52(8) . . ?
C7 N2 Mo1 107.83(8) . 3_666 ?
C7 N2 C11 111.35(11) . . ?
C7 N2 C9 110.60(10) . . ?
C11 N2 Mo1 108.32(8) . 3_666 ?
C11 N2 C9 111.47(11) . . ?
C9 N2 Mo1 107.08(9) . 3_666 ?
O12 C10 C9 116.35(13) . . ?
O13 C10 O12 125.47(15) . . ?
O13 C10 C9 118.12(14) . . ?
O10 C8 C7 112.66(11) . . ?
O11 C8 O10 125.68(14) . . ?
O11 C8 C7 121.66(12) . . ?
O14 C12 C11 117.24(11) . . ?
O15 C12 O14 123.28(13) . . ?
O15 C12 C11 119.44(14) . . ?
N2 C7 C8 115.69(11) . . ?
O5 C6 C5 116.68(13) . . ?
O6 C6 O5 124.12(14) . . ?
O6 C6 C5 119.19(13) . . ?
O1 C2 C1 115.13(12) . . ?
O2 C2 O1 124.89(14) . . ?
O2 C2 C1 119.97(13) . . ?
O3 C4 C3 117.32(12) . . ?
O4 C4 O3 124.92(13) . . ?
O4 C4 C3 117.76(14) . . ?
N2 C11 C12 112.47(12) . . ?
N2 C9 C10 112.35(12) . . ?
N1 C1 C2 109.34(11) . . ?
N1 C5 C6 108.63(11) . . ?
N1 C3 C4 112.66(12) . . ?
Na4 O8W Na4 122.78(9) . 3_565 ?
O15 Na4 Na2 67.28(7) 3_565 4_575 ?
O15 Na4 O8W 51.34(6) 3_565 3_565 ?
O8W Na4 Na2 82.97(8) 3_565 4_575 ?
O8W Na4 Na2 128.62(14) . 4_575 ?
O8W Na4 O15 102.52(12) . 3_565 ?
O8W Na4 O8W 57.22(9) . 3_565 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.171
_oxdiff_exptl_absorpt_empirical_full_min 0.906
