# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_rmk_219_e_scale
_database_code_depnum_ccdc_archive 'CCDC 2145351'
loop_
_audit_author_name
_audit_author_address
'Ryan M. Kirk'
;The Australian National University 
Australia
;
_audit_update_record             
;
2022-01-29 deposited with the CCDC.	2024-06-27 downloaded from the CCDC.
;
_audit_creation_date             2022-01-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H20 As Mo O3, C F3 O3 S'
_chemical_formula_sum            'C18 H20 As F3 Mo O6 S'
_chemical_formula_weight         592.26
_chemical_melting_point          ?
_chemical_oxdiff_formula         S1F3Mo1As1O6C18H20
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2247(2)
_cell_length_b                   8.7800(3)
_cell_length_c                   15.8527(5)
_cell_angle_alpha                98.816(2)
_cell_angle_beta                 95.151(2)
_cell_angle_gamma                93.888(2)
_cell_volume                     1122.80(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3840
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.3410
_cell_measurement_theta_min      5.1080
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.804
_exptl_absorpt_correction_T_max  0.59151
_exptl_absorpt_correction_T_min  0.55803
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 5 -6 0.0387
-5 -1 4 0.0636
4 -3 1 0.0536
1 -5 6 0.0675
-1 1 10 0.0215
0 0 -10 0.0165

_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.046
_exptl_crystal_size_rad          0.051
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.3935 4.9642 -6.2947 -0.0264 0.0282 -0.9993
-4.9242 -0.9875 4.3320 0.6696 -0.6353 0.3847
4.4337 -3.4142 1.3394 -0.6268 0.5919 0.5067
0.8624 -5.1094 5.6733 -0.1466 0.1357 0.9798
-0.7644 0.7765 9.8531 -0.4031 -0.8454 0.3504
0.2635 -0.1979 -10.0926 0.4677 0.7671 -0.4391

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8310
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.635
_diffrn_reflns_theta_min         5.115
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  56.00   1.00    3.93    --   37.17 -38.00-180.00   88
  2  ω     53.00 102.00   1.00    3.93    --   37.17  57.00  90.00   49
  3  ω     32.00  91.00   1.00    3.93    --   37.17-125.00-120.00   59
  4  ω     14.00  51.00   1.00    3.93    --   37.17 -57.00  90.00   37
  5  ω    -19.00  33.00   1.00    3.93    --   37.17 -77.00 -90.00   52
  6  ω    -20.00  61.00   1.00    3.93    --   37.17 -77.00  30.00   81
  7  ω     17.00  74.00   1.00    3.93    --   37.17 -99.00 -30.00   57
  8  ω     11.00 101.00   1.00    3.93    --   37.17  19.00  30.00   90
  9  ω     43.00 123.00   1.00   15.74    --  111.00 -50.00 -90.00   80
 10  ω     67.00 106.00   1.00   15.74    --  111.00 -92.00 150.00   39
 11  ω    105.00 132.00   1.00   15.74    --  111.00 -77.00-180.00   27
 12  ω     42.00 103.00   1.00   15.74    --  111.00-111.00 -60.00   61
 13  ω     95.00 171.00   1.00   15.74    --  111.00  50.00 120.00   76
 14  ω    119.00 172.00   1.00   15.74    --  111.00  77.00  60.00   53
 15  ω     60.00 105.00   1.00   15.74    --  111.00-111.00 -90.00   45
 16  ω     41.00 109.00   1.00   15.74    --  111.00-111.00 120.00   68
 17  ω     74.00 108.00   1.00   15.74    --  111.00-111.00 -30.00   34
 18  ω    152.00 178.00   1.00   15.74    --  111.00 111.00-180.00   26
 19  ω     49.00 126.00   1.00   15.74    --  111.00 -38.00 -30.00   77
 20  ω    107.00 136.00   1.00   15.74    --  111.00 111.00-180.00   29
 21  ω     42.00 109.00   1.00   15.74    --  111.00-111.00  30.00   67
 22  ω     63.00 115.00   1.00   15.74    --  111.00 -50.00  60.00   52
 23  ω     44.00 130.00   1.00   15.74    --  111.00 -38.00 120.00   86
 24  ω    115.00 176.00   1.00   15.74    --  111.00  77.00 -90.00   61
 25  ω     55.00  92.00   1.00   15.74    --  111.00 -77.00-180.00   37
 26  ω     56.00 178.00   1.00   15.74    --  111.00   0.00  60.00  122
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1686559000
_diffrn_orient_matrix_UB_12      -0.0549185000
_diffrn_orient_matrix_UB_13      -0.0496648000
_diffrn_orient_matrix_UB_21      0.0841861000
_diffrn_orient_matrix_UB_22      -0.0922883000
_diffrn_orient_matrix_UB_23      -0.0720012000
_diffrn_orient_matrix_UB_31      -0.0091014000
_diffrn_orient_matrix_UB_32      -0.1421702000
_diffrn_orient_matrix_UB_33      0.0460560000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3954
_reflns_number_total             4447
_reflns_odcompleteness_completeness 96.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.207
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4447
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0331
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0480P)²+0.1934P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0866
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C13(H13), C14(H14), C16(H16), C15(H15)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C)
;
_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 0.26513(3) 0.32167(3) 0.13826(2) 0.02512(9) Uani 1 1 d . . . . .
As1 As 0.10954(4) 0.43487(3) 0.26492(2) 0.02197(9) Uani 1 1 d . . . . .
S2 S 0.68203(10) -0.10430(10) 0.20573(6) 0.03532(18) Uani 1 1 d . . . . .
F1 F 0.5914(3) -0.2635(3) 0.32332(18) 0.0582(7) Uani 1 1 d . . . . .
F2 F 0.7900(4) -0.0902(4) 0.36869(18) 0.0758(10) Uani 1 1 d . . . . .
O1 O 0.5175(3) 0.3426(4) 0.30237(16) 0.0445(6) Uani 1 1 d . . . . .
F3 F 0.5437(4) -0.0228(4) 0.3471(2) 0.0724(9) Uani 1 1 d . . . . .
O5 O 0.8102(4) -0.2028(4) 0.1891(2) 0.0532(7) Uani 1 1 d . . . . .
O3 O 0.1661(4) 0.6311(4) 0.0796(2) 0.0532(7) Uani 1 1 d . . . . .
O4 O 0.5251(4) -0.1592(4) 0.1597(2) 0.0541(7) Uani 1 1 d . . . . .
O2 O 0.5938(4) 0.4402(5) 0.0723(2) 0.0640(10) Uani 1 1 d . . . . .
O6 O 0.7290(5) 0.0574(4) 0.2102(3) 0.0695(10) Uani 1 1 d . . . . .
C1 C 0.4274(4) 0.3388(4) 0.2435(2) 0.0322(7) Uani 1 1 d . . . . .
C7 C 0.1364(4) 0.3461(4) 0.3681(2) 0.0295(6) Uani 1 1 d . . . . .
C4 C 0.1832(4) 0.6343(4) 0.3301(2) 0.0318(7) Uani 1 1 d . . . . .
C6 C 0.1956(5) 0.4589(4) 0.4326(2) 0.0351(7) Uani 1 1 d . . . . .
C8 C -0.1243(4) 0.4401(4) 0.2360(2) 0.0318(6) Uani 1 1 d . . . . .
H8A H -0.142491 0.501365 0.191373 0.048 Uiso 1 1 calc R U . . .
H8B H -0.173079 0.484651 0.285842 0.048 Uiso 1 1 calc R U . . .
H8C H -0.172964 0.336700 0.216530 0.048 Uiso 1 1 calc R U . . .
C3 C 0.2062(5) 0.5237(4) 0.1053(2) 0.0360(7) Uani 1 1 d . . . . .
C5 C 0.2199(4) 0.6186(4) 0.4114(2) 0.0358(7) Uani 1 1 d . . . . .
C2 C 0.4759(5) 0.3993(6) 0.0964(2) 0.0454(9) Uani 1 1 d . . . . .
C17 C 0.0312(5) 0.1842(5) 0.0654(3) 0.0445(9) Uani 1 1 d . . . . .
H17 H -0.066460 0.231269 0.060980 0.053 Uiso 1 1 calc R U . . .
C9 C 0.1896(5) 0.7763(4) 0.2887(3) 0.0461(9) Uani 1 1 d . . . . .
H9A H 0.270745 0.769539 0.248702 0.069 Uiso 1 1 calc R U . . .
H9B H 0.217582 0.865755 0.331928 0.069 Uiso 1 1 calc R U . . .
H9C H 0.084457 0.784736 0.258961 0.069 Uiso 1 1 calc R U . . .
C12 C 0.1074(6) 0.1765(4) 0.3679(3) 0.0483(10) Uani 1 1 d . . . . .
H12A H -0.001261 0.141260 0.341952 0.072 Uiso 1 1 calc R U . . .
H12B H 0.118945 0.156208 0.425882 0.072 Uiso 1 1 calc R U . . .
H12C H 0.185819 0.123028 0.335896 0.072 Uiso 1 1 calc R U . . .
C13 C 0.0839(5) 0.1021(4) 0.1308(2) 0.0435(9) Uani 1 1 d . . . . .
H13 H 0.026349 0.084997 0.176875 0.052 Uiso 1 1 calc R U . . .
C18 C 0.6501(5) -0.1211(5) 0.3165(3) 0.0472(9) Uani 1 1 d . . . . .
C10 C 0.2832(7) 0.7496(5) 0.4824(3) 0.0599(12) Uani 1 1 d . . . . .
H10A H 0.297449 0.843620 0.458952 0.090 Uiso 1 1 calc R U . . .
H10B H 0.386443 0.727057 0.508956 0.090 Uiso 1 1 calc R U . . .
H10C H 0.206019 0.761574 0.524426 0.090 Uiso 1 1 calc R U . . .
C14 C 0.2376(6) 0.0504(4) 0.1152(3) 0.0522(11) Uani 1 1 d . . . . .
H14 H 0.300617 -0.006553 0.148612 0.063 Uiso 1 1 calc R U . . .
C16 C 0.1484(6) 0.1829(5) 0.0092(2) 0.0497(10) Uani 1 1 d . . . . .
H16 H 0.143162 0.228217 -0.040241 0.060 Uiso 1 1 calc R U . . .
C11 C 0.2386(7) 0.4316(6) 0.5230(3) 0.0585(12) Uani 1 1 d . . . . .
H11A H 0.215090 0.324114 0.526205 0.088 Uiso 1 1 calc R U . . .
H11B H 0.174972 0.492863 0.561072 0.088 Uiso 1 1 calc R U . . .
H11C H 0.352990 0.460370 0.539581 0.088 Uiso 1 1 calc R U . . .
C15 C 0.2782(6) 0.1017(5) 0.0386(3) 0.0597(12) Uani 1 1 d . . . . .
H15 H 0.373641 0.084813 0.012470 0.072 Uiso 1 1 calc R U . . .


_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 As1 2.5844(4) . ?
Mo1 C1 2.020(3) . ?
Mo1 C3 2.003(4) . ?
Mo1 C2 2.024(4) . ?
Mo1 C17 2.313(4) . ?
Mo1 C13 2.337(4) . ?
Mo1 C14 2.346(4) . ?
Mo1 C16 2.306(4) . ?
Mo1 C15 2.315(4) . ?
As1 C7 1.918(3) . ?
As1 C4 1.920(3) . ?
As1 C8 1.942(3) . ?
S2 O5 1.425(3) . ?
S2 O4 1.439(3) . ?
S2 O6 1.435(3) . ?
S2 C18 1.825(4) . ?
F1 C18 1.333(5) . ?
F2 C18 1.342(5) . ?
O1 C1 1.133(4) . ?
F3 C18 1.341(6) . ?
O3 C3 1.139(5) . ?
O2 C2 1.130(5) . ?
C7 C6 1.341(5) . ?
C7 C12 1.491(5) . ?
C4 C5 1.328(5) . ?
C4 C9 1.495(5) . ?
C6 C5 1.496(5) . ?
C6 C11 1.505(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C5 C10 1.509(5) . ?
C17 H17 0.9300 . ?
C17 C13 1.405(6) . ?
C17 C16 1.370(6) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9300 . ?
C13 C14 1.402(6) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C14 H14 0.9300 . ?
C14 C15 1.418(7) . ?
C16 H16 0.9300 . ?
C16 C15 1.408(7) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C15 H15 0.9300 . ?

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
C1 Mo1 As1 74.87(9) . . ?
C1 Mo1 C2 77.41(14) . . ?
C1 Mo1 C17 144.09(14) . . ?
C1 Mo1 C13 109.20(14) . . ?
C1 Mo1 C14 94.30(14) . . ?
C1 Mo1 C16 149.38(15) . . ?
C1 Mo1 C15 114.02(17) . . ?
C3 Mo1 As1 77.95(10) . . ?
C3 Mo1 C1 115.08(14) . . ?
C3 Mo1 C2 78.36(16) . . ?
C3 Mo1 C17 94.16(15) . . ?
C3 Mo1 C13 125.49(16) . . ?
C3 Mo1 C14 150.62(15) . . ?
C3 Mo1 C16 92.79(15) . . ?
C3 Mo1 C15 122.87(17) . . ?
C2 Mo1 As1 130.97(13) . . ?
C2 Mo1 C17 131.42(16) . . ?
C2 Mo1 C13 143.04(17) . . ?
C2 Mo1 C14 110.26(19) . . ?
C2 Mo1 C16 97.34(17) . . ?
C2 Mo1 C15 85.56(19) . . ?
C17 Mo1 As1 92.60(11) . . ?
C17 Mo1 C13 35.17(15) . . ?
C17 Mo1 C14 58.61(15) . . ?
C17 Mo1 C15 58.36(16) . . ?
C13 Mo1 As1 84.73(10) . . ?
C13 Mo1 C14 34.84(16) . . ?
C14 Mo1 As1 111.42(13) . . ?
C16 Mo1 As1 126.06(13) . . ?
C16 Mo1 C17 34.50(16) . . ?
C16 Mo1 C13 57.95(15) . . ?
C16 Mo1 C14 58.79(15) . . ?
C16 Mo1 C15 35.47(17) . . ?
C15 Mo1 As1 142.87(13) . . ?
C15 Mo1 C13 58.16(16) . . ?
C15 Mo1 C14 35.42(18) . . ?
C7 As1 Mo1 117.40(10) . . ?
C7 As1 C4 89.38(15) . . ?
C7 As1 C8 106.97(14) . . ?
C4 As1 Mo1 119.76(10) . . ?
C4 As1 C8 105.77(14) . . ?
C8 As1 Mo1 114.35(10) . . ?
O5 S2 O4 115.1(2) . . ?
O5 S2 O6 114.5(2) . . ?
O5 S2 C18 102.5(2) . . ?
O4 S2 C18 103.04(19) . . ?
O6 S2 O4 115.8(2) . . ?
O6 S2 C18 103.2(2) . . ?
O1 C1 Mo1 177.5(3) . . ?
C6 C7 As1 108.2(2) . . ?
C6 C7 C12 129.5(3) . . ?
C12 C7 As1 122.1(3) . . ?
C5 C4 As1 108.8(2) . . ?
C5 C4 C9 130.0(3) . . ?
C9 C4 As1 121.2(3) . . ?
C7 C6 C5 117.0(3) . . ?
C7 C6 C11 123.4(4) . . ?
C5 C6 C11 119.6(3) . . ?
As1 C8 H8A 109.5 . . ?
As1 C8 H8B 109.5 . . ?
As1 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O3 C3 Mo1 173.7(3) . . ?
C4 C5 C6 116.7(3) . . ?
C4 C5 C10 124.5(4) . . ?
C6 C5 C10 118.8(4) . . ?
O2 C2 Mo1 178.8(5) . . ?
Mo1 C17 H17 120.1 . . ?
C13 C17 Mo1 73.3(2) . . ?
C13 C17 H17 125.9 . . ?
C16 C17 Mo1 72.5(2) . . ?
C16 C17 H17 125.9 . . ?
C16 C17 C13 108.3(4) . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Mo1 C13 H13 121.6 . . ?
C17 C13 Mo1 71.5(2) . . ?
C17 C13 H13 125.7 . . ?
C14 C13 Mo1 72.9(2) . . ?
C14 C13 C17 108.7(4) . . ?
C14 C13 H13 125.7 . . ?
F1 C18 S2 111.5(3) . . ?
F1 C18 F2 106.9(4) . . ?
F1 C18 F3 107.7(3) . . ?
F2 C18 S2 111.8(3) . . ?
F3 C18 S2 111.3(3) . . ?
F3 C18 F2 107.4(4) . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Mo1 C14 H14 121.8 . . ?
C13 C14 Mo1 72.2(2) . . ?
C13 C14 H14 126.7 . . ?
C13 C14 C15 106.6(4) . . ?
C15 C14 Mo1 71.1(2) . . ?
C15 C14 H14 126.7 . . ?
Mo1 C16 H16 120.4 . . ?
C17 C16 Mo1 73.0(2) . . ?
C17 C16 H16 125.7 . . ?
C17 C16 C15 108.7(4) . . ?
C15 C16 Mo1 72.6(2) . . ?
C15 C16 H16 125.7 . . ?
C6 C11 H11A 109.5 . . ?
C6 C11 H11B 109.5 . . ?
C6 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Mo1 C15 H15 120.3 . . ?
C14 C15 Mo1 73.5(2) . . ?
C14 C15 H15 126.1 . . ?
C16 C15 Mo1 71.9(2) . . ?
C16 C15 C14 107.8(4) . . ?
C16 C15 H15 126.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 C17 C13 C14 -63.9(3) . . . . ?
Mo1 C17 C16 C15 64.4(3) . . . . ?
Mo1 C13 C14 C15 -63.2(3) . . . . ?
Mo1 C14 C15 C16 -64.2(3) . . . . ?
Mo1 C16 C15 C14 65.2(3) . . . . ?
As1 C7 C6 C5 2.0(4) . . . . ?
As1 C7 C6 C11 -177.6(3) . . . . ?
As1 C4 C5 C6 -0.5(4) . . . . ?
As1 C4 C5 C10 179.6(3) . . . . ?
O5 S2 C18 F1 -66.2(4) . . . . ?
O5 S2 C18 F2 53.5(4) . . . . ?
O5 S2 C18 F3 173.6(3) . . . . ?
O4 S2 C18 F1 53.7(4) . . . . ?
O4 S2 C18 F2 173.3(3) . . . . ?
O4 S2 C18 F3 -66.5(3) . . . . ?
O6 S2 C18 F1 174.6(3) . . . . ?
O6 S2 C18 F2 -65.8(4) . . . . ?
O6 S2 C18 F3 54.4(3) . . . . ?
C7 C6 C5 C4 -1.1(5) . . . . ?
C7 C6 C5 C10 178.8(4) . . . . ?
C17 C13 C14 Mo1 63.0(3) . . . . ?
C17 C13 C14 C15 -0.2(4) . . . . ?
C17 C16 C15 Mo1 -64.6(3) . . . . ?
C17 C16 C15 C14 0.6(5) . . . . ?
C9 C4 C5 C6 178.3(3) . . . . ?
C9 C4 C5 C10 -1.6(7) . . . . ?
C12 C7 C6 C5 176.5(4) . . . . ?
C12 C7 C6 C11 -3.0(6) . . . . ?
C13 C17 C16 Mo1 -65.1(3) . . . . ?
C13 C17 C16 C15 -0.7(5) . . . . ?
C13 C14 C15 Mo1 64.0(3) . . . . ?
C13 C14 C15 C16 -0.2(5) . . . . ?
C16 C17 C13 Mo1 64.5(3) . . . . ?
C16 C17 C13 C14 0.6(4) . . . . ?
C11 C6 C5 C4 178.5(4) . . . . ?
C11 C6 C5 C10 -1.6(6) . . . . ?


_ins_header                      
;
TITL RMK_219_E_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   8.224652   8.780038  15.852747  98.8163  95.1513  93.8883
ZERR    2.00   0.000244   0.000255   0.000478   0.0025   0.0024   0.0024
LATT  1
SFAC C H O F S As Mo
UNIT 36.00 40.00 12.00 6.00 2.00 2.00 2.00
TREF
HKLF 4
END
;
_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 1.347
_oxdiff_exptl_absorpt_empirical_full_min 0.812
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Et2O'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_rmk_219_c_red_b2_scale
_database_code_depnum_ccdc_archive 'CCDC 2145382'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2022-01-29 deposited with the CCDC.	2024-06-27 downloaded from the CCDC.
;
_audit_creation_date             2022-01-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H5 I Mo O3'
_chemical_formula_sum            'C8 H5 I Mo O3'
_chemical_formula_weight         371.96
_chemical_melting_point          ?
_chemical_oxdiff_formula         MoIC8H5
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   10.4658(3)
_cell_length_b                   7.8509(2)
_cell_length_c                   12.0747(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.736(2)
_cell_angle_gamma                90
_cell_volume                     992.05(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2189
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.1050
_cell_measurement_theta_min      5.5530
_shelx_estimated_absorpt_T_max   0.181
_shelx_estimated_absorpt_T_min   0.054
_exptl_absorpt_coefficient_mu    35.053
_exptl_absorpt_correction_T_max  0.61017
_exptl_absorpt_correction_T_min  0.57918
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.490
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             688
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 8 0.1053
6 3 1 0.0963
-1 0 -8 0.0509
-6 -3 -1 0.0263
-5 4 0 0.0147
5 -4 0 0.0552

_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.074
_exptl_crystal_size_rad          0.070
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.6308 -0.2604 7.7816 0.5911 0.1122 -0.7988
5.5896 2.8162 0.9673 0.8793 0.1628 0.4476
-1.0303 0.0500 -7.7294 -0.6461 -0.1223 0.7534
-5.5794 -2.7977 -1.1426 -0.8890 -0.1647 -0.4272
-4.7314 3.6562 -0.2016 -0.0251 -0.9996 0.0091
4.6326 -3.7177 0.4178 0.0252 0.9988 -0.0424

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3425
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.224
_diffrn_reflns_theta_min         5.559
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -97.00 -22.00   1.00    1.00    --  -36.18 -57.00  60.00   75
  2  ω    -12.00  33.00   1.00    1.00    --  -36.18  38.00-120.00   45
  3  ω     19.00  81.00   1.00    1.00    --   36.18  57.00   0.00   62
  4  ω     27.00  90.00   1.00    1.00    --   36.18-125.00 -90.00   63
  5  ω    141.00 174.00   1.00    1.00    --  109.99 111.00 -30.00   33
  6  ω    103.00 162.00   1.00    1.00    --  109.99  77.00 -90.00   59
  7  ω    104.00 170.00   1.00    1.00    --  109.99  77.00 -60.00   66
  8  ω     92.00 131.00   1.00    1.00    --  109.99 -30.00 150.00   39
  9  ω     41.00  85.00   1.00    1.00    --  109.99 -95.00 150.00   44
 10  ω    106.00 137.00   1.00    1.00    --  109.99 111.00 -30.00   31
 11  ω    111.00 168.00   1.00    1.00    --  109.99  77.00-180.00   57
 12  ω     40.00  84.00   1.00    1.00    --  109.99 -30.00 150.00   44
 13  ω     48.00 101.00   1.00    1.00    --  109.99 -95.00  60.00   53
 14  ω     96.00 177.00   1.00    1.00    --  109.99  61.00-120.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0885041000
_diffrn_orient_matrix_UB_12      0.1116526000
_diffrn_orient_matrix_UB_13      0.0725172000
_diffrn_orient_matrix_UB_21      0.1008368000
_diffrn_orient_matrix_UB_22      -0.1428387000
_diffrn_orient_matrix_UB_23      0.0014631000
_diffrn_orient_matrix_UB_31      0.0604838000
_diffrn_orient_matrix_UB_32      0.0749780000
_diffrn_orient_matrix_UB_33      -0.1050453000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1845
_reflns_number_total             1924
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.289
_refine_diff_density_min         -2.023
_refine_diff_density_rms         0.286
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1924
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0464
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0861P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1216
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C4(H4), C8(H8), C5(H5)
;
_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
I1 I 0.27314(4) 0.56947(5) 0.88025(3) 0.02668(19) Uani 1 1 d . . . . .
Mo1 Mo 0.48849(4) 0.54226(5) 0.74035(4) 0.01382(18) Uani 1 1 d . . . . .
O2 O 0.5565(4) 0.2481(6) 0.5765(4) 0.0273(9) Uani 1 1 d . . . . .
O1 O 0.2532(5) 0.5440(6) 0.5737(4) 0.0310(11) Uani 1 1 d . . . . .
O3 O 0.5115(5) 0.2165(6) 0.8912(4) 0.0310(10) Uani 1 1 d . . . . .
C3 C 0.4990(5) 0.3330(8) 0.8379(5) 0.0197(11) Uani 1 1 d . . . . .
C2 C 0.5329(5) 0.3563(8) 0.6354(5) 0.0190(11) Uani 1 1 d . . . . .
C1 C 0.3348(6) 0.5395(8) 0.6354(5) 0.0204(12) Uani 1 1 d . . . . .
C7 C 0.6946(5) 0.6368(8) 0.7524(6) 0.0274(14) Uani 1 1 d . . . . .
H7 H 0.761615 0.558958 0.752143 0.033 Uiso 1 1 calc R U . . .
C6 C 0.6375(6) 0.7109(9) 0.6585(6) 0.0295(15) Uani 1 1 d . . . . .
H6 H 0.658782 0.689224 0.585271 0.035 Uiso 1 1 calc R U . . .
C4 C 0.5391(7) 0.8163(9) 0.8091(8) 0.0396(19) Uani 1 1 d . . . . .
H4 H 0.483741 0.877848 0.853512 0.048 Uiso 1 1 calc R U . . .
C8 C 0.6338(7) 0.6997(9) 0.8467(6) 0.0327(16) Uani 1 1 d . . . . .
H8 H 0.652032 0.670694 0.919898 0.039 Uiso 1 1 calc R U . . .
C5 C 0.5438(7) 0.8223(8) 0.6939(7) 0.0357(17) Uani 1 1 d . . . . .
H5 H 0.492483 0.889800 0.648328 0.043 Uiso 1 1 calc R U . . .


_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
I1 Mo1 2.8419(6) . ?
Mo1 C3 2.024(6) . ?
Mo1 C2 1.992(6) . ?
Mo1 C1 2.035(6) . ?
Mo1 C7 2.284(6) . ?
Mo1 C6 2.281(6) . ?
Mo1 C4 2.364(6) . ?
Mo1 C8 2.333(6) . ?
Mo1 C5 2.343(6) . ?
O2 C2 1.137(8) . ?
O1 C1 1.126(8) . ?
O3 C3 1.125(8) . ?
C7 H7 0.9300 . ?
C7 C6 1.401(10) . ?
C7 C8 1.402(10) . ?
C6 H6 0.9300 . ?
C6 C5 1.386(11) . ?
C4 H4 0.9300 . ?
C4 C8 1.419(11) . ?
C4 C5 1.393(12) . ?
C8 H8 0.9300 . ?
C5 H5 0.9300 . ?

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
C3 Mo1 I1 75.69(16) . . ?
C3 Mo1 C1 113.0(2) . . ?
C3 Mo1 C7 100.5(2) . . ?
C3 Mo1 C6 133.7(2) . . ?
C3 Mo1 C4 121.6(3) . . ?
C3 Mo1 C8 94.6(2) . . ?
C3 Mo1 C5 152.8(2) . . ?
C2 Mo1 I1 128.80(16) . . ?
C2 Mo1 C3 76.3(2) . . ?
C2 Mo1 C1 77.6(2) . . ?
C2 Mo1 C7 92.9(2) . . ?
C2 Mo1 C6 89.0(2) . . ?
C2 Mo1 C4 146.9(2) . . ?
C2 Mo1 C8 125.6(3) . . ?
C2 Mo1 C5 118.4(3) . . ?
C1 Mo1 I1 75.19(19) . . ?
C1 Mo1 C7 141.4(3) . . ?
C1 Mo1 C6 106.0(2) . . ?
C1 Mo1 C4 113.6(3) . . ?
C1 Mo1 C8 148.5(3) . . ?
C1 Mo1 C5 93.2(2) . . ?
C7 Mo1 I1 133.90(19) . . ?
C7 Mo1 C4 58.3(2) . . ?
C7 Mo1 C8 35.3(3) . . ?
C7 Mo1 C5 58.3(2) . . ?
C6 Mo1 I1 139.98(19) . . ?
C6 Mo1 C7 35.8(2) . . ?
C6 Mo1 C4 58.2(3) . . ?
C6 Mo1 C8 59.1(2) . . ?
C6 Mo1 C5 34.8(3) . . ?
C4 Mo1 I1 84.19(17) . . ?
C8 Mo1 I1 98.59(19) . . ?
C8 Mo1 C4 35.2(3) . . ?
C8 Mo1 C5 58.2(2) . . ?
C5 Mo1 I1 105.8(2) . . ?
C5 Mo1 C4 34.4(3) . . ?
O3 C3 Mo1 176.4(5) . . ?
O2 C2 Mo1 178.6(5) . . ?
O1 C1 Mo1 176.3(6) . . ?
Mo1 C7 H7 119.8 . . ?
C6 C7 Mo1 72.0(3) . . ?
C6 C7 H7 125.7 . . ?
C6 C7 C8 108.5(6) . . ?
C8 C7 Mo1 74.2(3) . . ?
C8 C7 H7 125.7 . . ?
Mo1 C6 H6 118.6 . . ?
C7 C6 Mo1 72.3(3) . . ?
C7 C6 H6 126.0 . . ?
C5 C6 Mo1 75.0(4) . . ?
C5 C6 C7 108.0(6) . . ?
C5 C6 H6 126.0 . . ?
Mo1 C4 H4 122.5 . . ?
C8 C4 Mo1 71.2(4) . . ?
C8 C4 H4 126.0 . . ?
C5 C4 Mo1 72.0(4) . . ?
C5 C4 H4 126.0 . . ?
C5 C4 C8 107.9(6) . . ?
Mo1 C8 H8 121.2 . . ?
C7 C8 Mo1 70.5(3) . . ?
C7 C8 C4 106.8(6) . . ?
C7 C8 H8 126.6 . . ?
C4 C8 Mo1 73.6(4) . . ?
C4 C8 H8 126.6 . . ?
Mo1 C5 H5 122.3 . . ?
C6 C5 Mo1 70.1(4) . . ?
C6 C5 C4 108.7(6) . . ?
C6 C5 H5 125.6 . . ?
C4 C5 Mo1 73.6(4) . . ?
C4 C5 H5 125.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 C7 C6 C5 67.1(4) . . . . ?
Mo1 C7 C8 C4 -65.2(4) . . . . ?
Mo1 C6 C5 C4 63.9(5) . . . . ?
Mo1 C4 C8 C7 63.0(4) . . . . ?
Mo1 C4 C5 C6 -61.7(4) . . . . ?
C7 C6 C5 Mo1 -65.3(4) . . . . ?
C7 C6 C5 C4 -1.3(7) . . . . ?
C6 C7 C8 Mo1 64.3(4) . . . . ?
C6 C7 C8 C4 -0.8(7) . . . . ?
C8 C7 C6 Mo1 -65.8(4) . . . . ?
C8 C7 C6 C5 1.4(7) . . . . ?
C8 C4 C5 Mo1 62.5(4) . . . . ?
C8 C4 C5 C6 0.8(7) . . . . ?
C5 C4 C8 Mo1 -63.0(5) . . . . ?
C5 C4 C8 C7 0.0(7) . . . . ?


_ins_header                      
;
TITL RMK_219_C_red_b2_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  10.465832   7.850881  12.074665  90.0000  90.7358  90.0000
ZERR    6.00   0.000254   0.000186   0.000295   0.0000   0.0021   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H Mo I
UNIT 48.00 30.00 6.00 6.00
TREF
HKLF 4
END
;
_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 2.385
_oxdiff_exptl_absorpt_empirical_full_min 0.521
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-hexane'
####################################################################### 
# 
# 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_rmk_223_c_scale
_database_code_depnum_ccdc_archive 'CCDC 2145459'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2022-01-30 deposited with the CCDC.	2024-06-27 downloaded from the CCDC.
;
_audit_creation_date             2022-01-30
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H24 As Mo O3 Si, C F3 O3 S'
_chemical_formula_sum            'C19 H24 As F3 Mo O6 S Si'
_chemical_formula_weight         636.39
_chemical_melting_point          ?
_chemical_oxdiff_formula         C19H24As1F3Mo1O6S1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 '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                   16.9991(3)
_cell_length_b                   23.3532(3)
_cell_length_c                   7.29480(10)
_cell_angle_alpha                90
_cell_angle_beta                 119.920(3)
_cell_angle_gamma                90
_cell_volume                     2509.95(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5795
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.4980
_cell_measurement_theta_min      5.9730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.470
_exptl_absorpt_correction_T_max  0.54879
_exptl_absorpt_correction_T_min  0.51041
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1272
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 12 0 0.0347
-6 -12 0 0.0490
9 5 -4 0.0626
-8 -1 5 0.1016
9 -6 0 0.0442
-9 7 1 0.0318

_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.087
_exptl_crystal_size_rad          0.065
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5.9276 11.5708 0.2018 -0.6202 0.5855 -0.5221
-5.6463 -11.6102 -0.3870 0.6046 -0.5706 0.5557
8.9786 4.7137 -3.9357 -0.6367 0.6046 0.4787
-7.8764 -0.8189 4.5503 0.4802 -0.4573 -0.7485
8.5377 -6.3047 0.1367 -0.8783 -0.4780 -0.0090
-8.9130 7.4590 0.5724 0.8661 0.4719 -0.1649

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9888
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.656
_diffrn_reflns_theta_min         4.832
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -27.00  -1.00   1.00    1.00    --   36.95 -57.00  30.00   26
  2  ω     31.00  75.00   1.00    1.00    --   36.95 -99.00-120.00   44
  3  ω      1.00  54.00   1.00    1.00    --   36.95 -57.00  30.00   53
  4  ω    -30.00  54.00   1.00    1.00    --   36.95 -57.00 -60.00   84
  5  ω     20.00 105.00   1.00    1.00    --   36.95  38.00-180.00   85
  6  ω    100.00 177.00   1.00    3.30    --  111.00  50.00 120.00   77
  7  ω    114.00 177.00   1.00    3.30    --  111.00  77.00  60.00   63
  8  ω     74.00 131.00   1.00    3.30    --  111.00 -64.00-120.00   57
  9  ω     43.00 118.00   1.00    3.30    --  111.00 -38.00 -30.00   75
 10  ω     43.00 126.00   1.00    3.30    --  111.00 -50.00  60.00   83
 11  ω    119.00 177.00   1.00    3.30    --  111.00 111.00   0.00   58
 12  ω     51.00 106.00   1.00    3.30    --  111.00 -92.00  30.00   55
 13  ω    110.00 178.00   1.00    3.30    --  111.00  38.00 150.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1018680000
_diffrn_orient_matrix_UB_12      -0.0001760000
_diffrn_orient_matrix_UB_13      -0.0708387000
_diffrn_orient_matrix_UB_21      -0.0112215000
_diffrn_orient_matrix_UB_22      0.0582545000
_diffrn_orient_matrix_UB_23      -0.1094414000
_diffrn_orient_matrix_UB_31      -0.0206302000
_diffrn_orient_matrix_UB_32      -0.0309689000
_diffrn_orient_matrix_UB_33      -0.2057850000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4570
_reflns_number_total             4964
_reflns_odcompleteness_completeness 96.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.504
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4964
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0411
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0607P)²+4.6537P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1108
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C16(H16), C17(H17), C18(H18), C4(H4)
2.b Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C10(H10a,H10b,H10c), C9(H9a,H9b,H9c), C12(H12a,H12b,H12c),
 C13(H13a,H13b,H13c), C11(H11a,H11b,H11c)
;
_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 0.76608(2) 0.46899(2) 0.61623(4) 0.02842(10) Uani 1 1 d . . . . .
As1 As 0.72550(3) 0.36442(2) 0.47738(6) 0.03029(12) Uani 1 1 d . . . . .
S1 S 0.95705(9) 0.62612(5) 0.4736(2) 0.0529(3) Uani 1 1 d . . . . .
Si1 Si 0.50058(8) 0.35653(6) 0.1429(2) 0.0529(3) Uani 1 1 d . . . . .
F1 F 0.8384(3) 0.70621(15) 0.2693(7) 0.0830(12) Uani 1 1 d . . . . .
F2 F 0.8302(3) 0.63380(18) 0.0814(6) 0.0899(12) Uani 1 1 d . . . . .
O3 O 0.7282(3) 0.48477(17) 0.1510(5) 0.0603(10) Uani 1 1 d . . . . .
O4 O 0.9498(4) 0.56513(16) 0.4474(8) 0.0796(14) Uani 1 1 d . . . . .
O6 O 1.0175(3) 0.6539(2) 0.4142(8) 0.0778(12) Uani 1 1 d . . . . .
F3 F 0.7819(3) 0.6279(2) 0.3049(8) 0.0944(13) Uani 1 1 d . . . . .
O5 O 0.9630(4) 0.6470(2) 0.6657(7) 0.0786(13) Uani 1 1 d . . . . .
C15 C 0.8748(3) 0.4429(2) 0.9569(6) 0.0417(9) Uani 1 1 d . . . . .
H15 H 0.861413 0.417090 1.034634 0.050 Uiso 1 1 calc R . . . .
O1 O 0.5987(3) 0.4443(3) 0.6772(7) 0.0890(17) Uani 1 1 d . . . . .
O2 O 0.6622(4) 0.58624(19) 0.4786(8) 0.0948(17) Uani 1 1 d . . . . .
C6 C 0.6177(3) 0.28951(18) 0.5198(7) 0.0397(9) Uani 1 1 d . . . . .
C7 C 0.6069(3) 0.33228(17) 0.3864(6) 0.0356(8) Uani 1 1 d . . . . .
C3 C 0.7390(3) 0.47801(18) 0.3162(7) 0.0433(9) Uani 1 1 d . . . . .
C14 C 0.9109(3) 0.4290(2) 0.8238(7) 0.0428(9) Uani 1 1 d . . . . .
H14 H 0.925464 0.392469 0.799572 0.051 Uiso 1 1 calc R . . . .
C16 C 0.8628(3) 0.5025(2) 0.9499(6) 0.0417(9) Uani 1 1 d . . . . .
H16 H 0.840275 0.523331 1.022342 0.050 Uiso 1 1 calc R . . . .
C17 C 0.8916(3) 0.52537(19) 0.8113(7) 0.0433(10) Uani 1 1 d . . . . .
H17 H 0.890855 0.563838 0.777466 0.052 Uiso 1 1 calc R . . . .
C18 C 0.9210(3) 0.4800(2) 0.7349(7) 0.0430(9) Uani 1 1 d . . . . .
H18 H 0.943260 0.483095 0.641937 0.052 Uiso 1 1 calc R . . . .
C8 C 0.7582(4) 0.3402(2) 0.2690(9) 0.0548(12) Uani 1 1 d . . . . .
H8A H 0.722166 0.360778 0.139356 0.082 Uiso 1 1 calc GR . . . .
H8B H 0.747398 0.299902 0.243559 0.082 Uiso 1 1 calc GR . . . .
H8C H 0.821334 0.348105 0.321104 0.082 Uiso 1 1 calc GR . . . .
C1 C 0.6580(3) 0.4522(2) 0.6498(7) 0.0498(11) Uani 1 1 d . . . . .
C5 C 0.7115(4) 0.27642(18) 0.6921(7) 0.0456(10) Uani 1 1 d . . . . .
C4 C 0.7770(3) 0.30848(19) 0.6975(7) 0.0469(10) Uani 1 1 d . . . . .
H4 H 0.838590 0.304373 0.793692 0.056 Uiso 1 1 calc R . . . .
C2 C 0.6992(4) 0.5436(2) 0.5290(8) 0.0575(13) Uani 1 1 d . . . . .
C19 C 0.8469(4) 0.6496(2) 0.2723(9) 0.0585(13) Uani 1 1 d . . . . .
C10 C 0.5402(4) 0.2532(2) 0.5002(9) 0.0588(13) Uani 1 1 d . . . . .
H10A H 0.483510 0.270599 0.401320 0.088 Uiso 1 1 calc GR . . . .
H10B H 0.544163 0.250186 0.635850 0.088 Uiso 1 1 calc GR . . . .
H10C H 0.543785 0.215641 0.451148 0.088 Uiso 1 1 calc GR . . . .
C9 C 0.7294(5) 0.2284(2) 0.8468(9) 0.0705(17) Uani 1 1 d . . . . .
H9A H 0.693710 0.234155 0.913902 0.106 Uiso 1 1 calc GR . . . .
H9B H 0.792587 0.227884 0.952030 0.106 Uiso 1 1 calc GR . . . .
H9C H 0.713122 0.192478 0.772622 0.106 Uiso 1 1 calc GR . . . .
C12 C 0.5162(8) 0.4275(5) 0.0635(18) 0.185(7) Uani 1 1 d . . . . .
H12A H 0.544318 0.452009 0.185264 0.278 Uiso 1 1 calc GR . . . .
H12B H 0.458253 0.443033 -0.037823 0.278 Uiso 1 1 calc GR . . . .
H12C H 0.554201 0.424909 0.001154 0.278 Uiso 1 1 calc GR . . . .
C13 C 0.4495(9) 0.3028(4) -0.0507(14) 0.210(9) Uani 1 1 d . . . . .
H13A H 0.495645 0.281051 -0.058397 0.315 Uiso 1 1 calc GR . . . .
H13B H 0.410314 0.320190 -0.185521 0.315 Uiso 1 1 calc GR . . . .
H13C H 0.414561 0.277921 -0.013854 0.315 Uiso 1 1 calc GR . . . .
C11 C 0.4156(9) 0.3801(9) 0.219(2) 0.260(13) Uani 1 1 d . . . . .
H11A H 0.437913 0.371543 0.365127 0.389 Uiso 1 1 calc GR . . . .
H11B H 0.359372 0.360357 0.133347 0.389 Uiso 1 1 calc GR . . . .
H11C H 0.405961 0.420645 0.196424 0.389 Uiso 1 1 calc GR . . . .


_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 As1 2.6017(5) . ?
Mo1 C15 2.319(4) . ?
Mo1 C3 2.010(5) . ?
Mo1 C14 2.347(4) . ?
Mo1 C16 2.291(4) . ?
Mo1 C17 2.298(4) . ?
Mo1 C18 2.340(4) . ?
Mo1 C1 2.010(5) . ?
Mo1 C2 2.003(5) . ?
As1 C7 1.932(4) . ?
As1 C8 1.945(4) . ?
As1 C4 1.910(4) . ?
S1 O4 1.434(4) . ?
S1 O6 1.453(5) . ?
S1 O5 1.439(4) . ?
S1 C19 1.794(6) . ?
Si1 C7 1.882(4) . ?
Si1 C12 1.818(11) . ?
Si1 C13 1.761(8) . ?
Si1 C11 1.868(14) . ?
F1 C19 1.329(6) . ?
F2 C19 1.327(7) . ?
O3 C3 1.136(6) . ?
F3 C19 1.341(7) . ?
C15 C14 1.421(6) . ?
C15 C16 1.404(7) . ?
O1 C1 1.135(6) . ?
O2 C2 1.136(6) . ?
C6 C7 1.342(6) . ?
C6 C5 1.489(7) . ?
C6 C10 1.512(6) . ?
C14 C18 1.407(7) . ?
C16 C17 1.428(6) . ?
C17 C18 1.400(6) . ?
C5 C4 1.326(7) . ?
C5 C9 1.511(6) . ?

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
C15 Mo1 As1 94.89(12) . . ?
C15 Mo1 C14 35.46(16) . . ?
C15 Mo1 C18 58.97(15) . . ?
C3 Mo1 As1 78.59(12) . . ?
C3 Mo1 C15 145.21(18) . . ?
C3 Mo1 C14 109.92(18) . . ?
C3 Mo1 C16 140.72(17) . . ?
C3 Mo1 C17 104.58(18) . . ?
C3 Mo1 C18 89.75(18) . . ?
C14 Mo1 As1 82.36(11) . . ?
C16 Mo1 As1 130.15(12) . . ?
C16 Mo1 C15 35.47(17) . . ?
C16 Mo1 C14 58.95(16) . . ?
C16 Mo1 C17 36.26(16) . . ?
C16 Mo1 C18 59.35(15) . . ?
C17 Mo1 As1 139.72(12) . . ?
C17 Mo1 C15 59.33(16) . . ?
C17 Mo1 C14 58.48(16) . . ?
C17 Mo1 C18 35.11(16) . . ?
C18 Mo1 As1 106.17(12) . . ?
C18 Mo1 C14 34.93(16) . . ?
C1 Mo1 As1 77.48(14) . . ?
C1 Mo1 C15 96.10(18) . . ?
C1 Mo1 C3 115.24(19) . . ?
C1 Mo1 C14 124.9(2) . . ?
C1 Mo1 C16 98.78(16) . . ?
C1 Mo1 C17 131.24(17) . . ?
C1 Mo1 C18 154.81(18) . . ?
C2 Mo1 As1 134.00(16) . . ?
C2 Mo1 C15 126.27(19) . . ?
C2 Mo1 C3 77.2(2) . . ?
C2 Mo1 C14 142.9(2) . . ?
C2 Mo1 C16 91.90(19) . . ?
C2 Mo1 C17 84.4(2) . . ?
C2 Mo1 C18 112.2(2) . . ?
C2 Mo1 C1 78.5(3) . . ?
C7 As1 Mo1 121.81(12) . . ?
C7 As1 C8 105.95(19) . . ?
C8 As1 Mo1 116.94(15) . . ?
C4 As1 Mo1 113.16(14) . . ?
C4 As1 C7 89.16(19) . . ?
C4 As1 C8 105.6(2) . . ?
O4 S1 O6 115.5(3) . . ?
O4 S1 O5 115.2(3) . . ?
O4 S1 C19 102.1(3) . . ?
O6 S1 C19 102.9(3) . . ?
O5 S1 O6 115.0(3) . . ?
O5 S1 C19 103.4(3) . . ?
C12 Si1 C7 110.5(3) . . ?
C12 Si1 C11 94.7(8) . . ?
C13 Si1 C7 113.6(3) . . ?
C13 Si1 C12 119.1(6) . . ?
C13 Si1 C11 107.6(8) . . ?
C11 Si1 C7 109.3(4) . . ?
C14 C15 Mo1 73.3(2) . . ?
C16 C15 Mo1 71.2(2) . . ?
C16 C15 C14 107.7(4) . . ?
C7 C6 C5 117.8(4) . . ?
C7 C6 C10 123.5(4) . . ?
C5 C6 C10 118.7(4) . . ?
Si1 C7 As1 123.6(2) . . ?
C6 C7 As1 107.4(3) . . ?
C6 C7 Si1 128.9(3) . . ?
O3 C3 Mo1 176.1(4) . . ?
C15 C14 Mo1 71.2(2) . . ?
C18 C14 Mo1 72.3(2) . . ?
C18 C14 C15 108.4(4) . . ?
C15 C16 Mo1 73.4(2) . . ?
C15 C16 C17 107.6(4) . . ?
C17 C16 Mo1 72.1(2) . . ?
C16 C17 Mo1 71.6(2) . . ?
C18 C17 Mo1 74.1(2) . . ?
C18 C17 C16 108.4(4) . . ?
C14 C18 Mo1 72.8(2) . . ?
C17 C18 Mo1 70.8(2) . . ?
C17 C18 C14 107.9(4) . . ?
O1 C1 Mo1 176.7(4) . . ?
C6 C5 C9 120.9(5) . . ?
C4 C5 C6 116.0(4) . . ?
C4 C5 C9 123.0(5) . . ?
C5 C4 As1 109.6(3) . . ?
O2 C2 Mo1 178.9(6) . . ?
F1 C19 S1 112.2(5) . . ?
F1 C19 F3 106.6(5) . . ?
F2 C19 S1 111.3(4) . . ?
F2 C19 F1 107.2(5) . . ?
F2 C19 F3 108.4(5) . . ?
F3 C19 S1 110.8(4) . . ?


_ins_header                      
;
TITL RMK_223_C_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  16.999093  23.353169   7.294825  90.0000 119.9198  90.0000
ZERR    4.00   0.000331   0.000316   0.000145   0.0000   0.0026   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H O F S As Mo
UNIT 76.00 96.00 24.00 12.00 4.00 4.00 4.00
TREF
HKLF 4
END
;
_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 1.275
_oxdiff_exptl_absorpt_empirical_full_min 0.745
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Et2O'
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_rmk_219_c_red_a_scale
_database_code_depnum_ccdc_archive 'CCDC 2145383'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2022-01-29 deposited with the CCDC.	2024-06-27 downloaded from the CCDC.
;
_audit_creation_date             2022-01-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H20 As I Mo O2'
_chemical_formula_sum            'C16 H20 As I Mo O2'
_chemical_formula_weight         542.08
_chemical_melting_point          ?
_chemical_oxdiff_formula         Mo1As1O3I1C16H20
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8572(3)
_cell_length_b                   13.9206(4)
_cell_length_c                   16.0715(5)
_cell_angle_alpha                104.867(3)
_cell_angle_beta                 104.316(3)
_cell_angle_gamma                91.742(2)
_cell_volume                     1846.43(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7113
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.1350
_cell_measurement_theta_min      5.1620
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    20.938
_exptl_absorpt_correction_T_max  0.50578
_exptl_absorpt_correction_T_min  0.46185
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1040
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -2 -9 0.0448
5 2 -5 0.0996
2 -8 1 0.0681
-3 8 0 0.0719
2 8 -6 0.0839
2 -9 3 0.0783
-1 4 8 0.1077
-3 -1 10 0.1094
-5 0 -1 0.1531
5 2 0 0.0840

_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.142
_exptl_crystal_size_rad          0.101
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.8349 -2.3614 -8.9578 0.4240 0.8922 -0.1554
5.4852 1.5978 -5.1456 0.9011 -0.0237 0.4330
2.3945 -8.2892 0.5881 0.6283 -0.0139 -0.7779
-2.5166 8.1996 -0.4566 -0.6469 0.0144 0.7624
1.5595 8.1568 -6.2227 0.1115 0.2286 0.9671
1.5111 -8.6714 3.4667 0.4375 -0.2105 -0.8742
-0.5300 4.0092 7.7038 -0.4031 -0.8454 0.3504
-3.4623 -1.2918 9.6020 -0.7137 -0.6097 -0.3448
-5.3211 -0.0319 -1.1954 -0.7750 0.5927 -0.2194
5.1687 2.4295 -0.0001 0.6999 -0.5344 0.4738

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11500
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.367
_diffrn_reflns_theta_min         3.781
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -86.00 -32.00   1.00    1.00    --  -36.18 125.00   0.00   54
  2  ω     -9.00  41.00   1.00    1.00    --   36.18 -38.00 120.00   50
  3  ω    -27.00  40.00   1.00    1.00    --   36.18 -57.00 -60.00   67
  4  ω     23.00 105.00   1.00    1.00    --   36.18  38.00  60.00   82
  5  ω     43.00  90.00   1.00    1.00    --   36.18-125.00-120.00   47
  6  ω    -22.00  44.00   1.00    1.00    --   36.18 -57.00  90.00   66
  7  ω     18.00 103.00   1.00    1.00    --   36.18  38.00 -90.00   85
  8  ω     42.00 126.00   1.00    1.00    --  109.99 -45.00  60.00   84
  9  ω     42.00 123.00   1.00    1.00    --  109.99 -45.00 -30.00   81
 10  ω     43.00 105.00   1.00    1.00    --  109.99 -61.00-120.00   62
 11  ω     42.00 106.00   1.00    1.00    --  109.99 -95.00   0.00   64
 12  ω     77.00 174.00   1.00    1.00    --  109.99  15.00 -30.00   97
 13  ω     40.00 109.00   1.00    1.00    --  109.99-111.00 -90.00   69
 14  ω     62.00 106.00   1.00    1.00    --  109.99 -95.00 150.00   44
 15  ω     58.00 131.00   1.00    1.00    --  109.99 -30.00-120.00   73
 16  ω     97.00 149.00   1.00    1.00    --  109.99  45.00  90.00   52
 17  ω    106.00 171.00   1.00    1.00    --  109.99 111.00 -30.00   65
 18  ω     98.00 176.00   1.00    1.00    --  109.99  61.00  30.00   78
 19  ω     46.00 109.00   1.00    1.00    --  109.99-111.00 120.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1513110000
_diffrn_orient_matrix_UB_12      -0.0338095000
_diffrn_orient_matrix_UB_13      -0.0243162000
_diffrn_orient_matrix_UB_21      -0.0888000000
_diffrn_orient_matrix_UB_22      -0.0310496000
_diffrn_orient_matrix_UB_23      -0.0996945000
_diffrn_orient_matrix_UB_31      0.0420646000
_diffrn_orient_matrix_UB_32      0.1055289000
_diffrn_orient_matrix_UB_33      -0.0065461000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6786
_reflns_number_total             7149
_reflns_odcompleteness_completeness 95.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.08
_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 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.133
_refine_diff_density_min         -1.637
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7149
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0355
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0535P)²+0.4711P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0927
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12B(H12B), C14A(H14A), C16B(H16B), C15B(H15B), C13A(H13A), C15A(H15A),
 C16A(H16A), C12A(H12A), C13B(H13B), C14B(H14B)
2.b Idealised Me refined as rotating group:
 C7B(H7BA,H7BB,H7BC), C10A(H10D,H10E,H10F), C8B(H8BA,H8BB,H8BC), C7A(H7AA,H7AB,
 H7AC), C11A(H11D,H11E,H11F), C8A(H8AA,H8AB,H8AC), C11B(H11A,H11B,H11C),
 C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC), C10B(H10A,H10B,H10C)
;
_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
I1B I 0.06429(3) 0.18689(2) 0.21370(2) 0.01949(8) Uani 1 1 d . . . . .
I1A I 0.27303(3) 0.67446(2) 0.16633(2) 0.01921(8) Uani 1 1 d . . . . .
Mo1A Mo 0.37438(4) 0.58044(2) 0.30595(2) 0.01207(9) Uani 1 1 d . . . . .
Mo1B Mo 0.23002(4) 0.09509(2) 0.34326(2) 0.01213(9) Uani 1 1 d . . . . .
As1A As 0.07574(5) 0.55696(3) 0.28042(3) 0.01300(11) Uani 1 1 d . . . . .
As1B As 0.38383(5) 0.05195(3) 0.22499(3) 0.01305(11) Uani 1 1 d . . . . .
O1A O 0.3369(5) 0.6380(3) 0.4964(2) 0.0269(8) Uani 1 1 d . . . . .
O1B O 0.5745(4) 0.1274(3) 0.4522(2) 0.0247(7) Uani 1 1 d . . . . .
O2A O 0.5666(5) 0.7903(2) 0.3866(2) 0.0281(8) Uani 1 1 d . . . . .
O2B O 0.2521(5) 0.3149(2) 0.4601(2) 0.0273(8) Uani 1 1 d . . . . .
C5A C -0.1415(5) 0.6735(3) 0.2273(3) 0.0162(8) Uani 1 1 d . . . . .
C6A C -0.0364(5) 0.6730(3) 0.3035(3) 0.0154(8) Uani 1 1 d . . . . .
C3A C -0.0612(5) 0.5136(3) 0.1609(3) 0.0189(9) Uani 1 1 d . . . . .
C4A C -0.1551(6) 0.5855(3) 0.1489(3) 0.0193(9) Uani 1 1 d . . . . .
C6B C 0.5121(6) 0.1519(3) 0.2030(3) 0.0198(9) Uani 1 1 d . . . . .
C7B C 0.5276(6) -0.0483(3) 0.2449(3) 0.0222(10) Uani 1 1 d . . . . .
H7BA H 0.596211 -0.025934 0.304062 0.033 Uiso 1 1 calc R U . . .
H7BB H 0.588409 -0.058160 0.202070 0.033 Uiso 1 1 calc R U . . .
H7BC H 0.468914 -0.110165 0.238294 0.033 Uiso 1 1 calc R U . . .
C5B C 0.4704(6) 0.1449(3) 0.1147(3) 0.0212(10) Uani 1 1 d . . . . .
C12B C 0.1108(6) -0.0716(3) 0.2937(3) 0.0246(10) Uani 1 1 d . . . . .
H12B H 0.118093 -0.116370 0.241134 0.029 Uiso 1 1 calc R U . . .
C14A C 0.5729(6) 0.4911(3) 0.3494(4) 0.0240(10) Uani 1 1 d . . . . .
H14A H 0.640852 0.515284 0.406115 0.029 Uiso 1 1 calc R U . . .
C16B C -0.0106(6) -0.0096(3) 0.3025(4) 0.0249(10) Uani 1 1 d . . . . .
H16B H -0.097296 -0.006640 0.257092 0.030 Uiso 1 1 calc R U . . .
C10A C -0.2463(6) 0.7550(3) 0.2175(4) 0.0250(10) Uani 1 1 d . . . . .
H10D H -0.225565 0.805628 0.273333 0.037 Uiso 1 1 calc R U . . .
H10E H -0.353766 0.727645 0.200299 0.037 Uiso 1 1 calc R U . . .
H10F H -0.226497 0.783910 0.172537 0.037 Uiso 1 1 calc R U . . .
C8B C 0.1550(6) -0.0770(4) 0.0621(3) 0.0250(10) Uani 1 1 d . . . . .
H8BA H 0.196402 -0.137561 0.071277 0.038 Uiso 1 1 calc R U . . .
H8BB H 0.113037 -0.085114 -0.000632 0.038 Uiso 1 1 calc R U . . .
H8BC H 0.073528 -0.062445 0.091916 0.038 Uiso 1 1 calc R U . . .
C15B C 0.0234(6) 0.0476(3) 0.3935(4) 0.0265(11) Uani 1 1 d . . . . .
H15B H -0.036314 0.095410 0.417801 0.032 Uiso 1 1 calc R U . . .
C13A C 0.4324(6) 0.4277(3) 0.3266(4) 0.0262(11) Uani 1 1 d . . . . .
H13A H 0.391324 0.403132 0.365856 0.031 Uiso 1 1 calc R U . . .
C2B C 0.2443(5) 0.2350(3) 0.4154(3) 0.0183(9) Uani 1 1 d . . . . .
C2A C 0.4934(6) 0.7149(3) 0.3566(3) 0.0189(9) Uani 1 1 d . . . . .
C15A C 0.5911(6) 0.5109(3) 0.2694(4) 0.0222(10) Uani 1 1 d . . . . .
H15A H 0.672627 0.551277 0.264835 0.027 Uiso 1 1 calc R U . . .
C16A C 0.4641(6) 0.4589(3) 0.1986(3) 0.0247(10) Uani 1 1 d . . . . .
H16A H 0.448447 0.458241 0.139042 0.030 Uiso 1 1 calc R U . . .
C3B C 0.2814(6) 0.0061(3) 0.0987(3) 0.0195(9) Uani 1 1 d . . . . .
C12A C 0.3647(6) 0.4080(3) 0.2329(4) 0.0269(11) Uani 1 1 d . . . . .
H12A H 0.271705 0.368669 0.200320 0.032 Uiso 1 1 calc R U . . .
C7A C 0.0078(6) 0.4715(3) 0.3456(3) 0.0221(9) Uani 1 1 d . . . . .
H7AA H 0.042698 0.503415 0.408532 0.033 Uiso 1 1 calc R U . . .
H7AB H 0.051488 0.408813 0.332618 0.033 Uiso 1 1 calc R U . . .
H7AC H -0.104468 0.460007 0.327932 0.033 Uiso 1 1 calc R U . . .
C4B C 0.3419(6) 0.0652(3) 0.0578(3) 0.0197(9) Uani 1 1 d . . . . .
C11A C -0.0017(6) 0.7449(3) 0.3934(3) 0.0250(10) Uani 1 1 d . . . . .
H11D H 0.107733 0.768313 0.413051 0.037 Uiso 1 1 calc R U . . .
H11E H -0.027831 0.712336 0.434654 0.037 Uiso 1 1 calc R U . . .
H11F H -0.062469 0.800467 0.390736 0.037 Uiso 1 1 calc R U . . .
C8A C -0.0441(7) 0.4196(4) 0.0957(4) 0.0318(12) Uani 1 1 d . . . . .
H8AA H -0.045266 0.364847 0.121783 0.048 Uiso 1 1 calc R U . . .
H8AB H 0.053220 0.426056 0.080519 0.048 Uiso 1 1 calc R U . . .
H8AC H -0.129296 0.407236 0.042792 0.048 Uiso 1 1 calc R U . . .
C11B C 0.6379(6) 0.2198(3) 0.2758(4) 0.0261(10) Uani 1 1 d . . . . .
H11A H 0.602186 0.240216 0.328855 0.039 Uiso 1 1 calc R U . . .
H11B H 0.662855 0.277602 0.257746 0.039 Uiso 1 1 calc R U . . .
H11C H 0.729631 0.185272 0.287751 0.039 Uiso 1 1 calc R U . . .
C1A C 0.3495(6) 0.6187(3) 0.4281(3) 0.0237(10) Uani 1 1 d . . . . .
C9A C -0.2714(7) 0.5814(4) 0.0618(3) 0.0309(12) Uani 1 1 d . . . . .
H9AA H -0.238952 0.632256 0.037499 0.046 Uiso 1 1 calc R U . . .
H9AB H -0.372729 0.592380 0.071848 0.046 Uiso 1 1 calc R U . . .
H9AC H -0.276795 0.517032 0.020596 0.046 Uiso 1 1 calc R U . . .
C1B C 0.4515(6) 0.1191(4) 0.4134(3) 0.0240(10) Uani 1 1 d . . . . .
C9B C 0.2889(7) 0.0538(4) -0.0408(3) 0.0326(12) Uani 1 1 d . . . . .
H9BA H 0.243564 0.112896 -0.051109 0.049 Uiso 1 1 calc R U . . .
H9BB H 0.212229 -0.002945 -0.068667 0.049 Uiso 1 1 calc R U . . .
H9BC H 0.377058 0.044252 -0.065770 0.049 Uiso 1 1 calc R U . . .
C13B C 0.2198(6) -0.0541(3) 0.3784(4) 0.0255(10) Uani 1 1 d . . . . .
H13B H 0.311299 -0.084821 0.391106 0.031 Uiso 1 1 calc R U . . .
C14B C 0.1645(7) 0.0186(4) 0.4403(3) 0.0268(11) Uani 1 1 d . . . . .
H14B H 0.212410 0.043006 0.501084 0.032 Uiso 1 1 calc R U . . .
C10B C 0.5451(8) 0.2098(4) 0.0721(4) 0.0374(14) Uani 1 1 d . . . . .
H10A H 0.623722 0.257223 0.117059 0.056 Uiso 1 1 calc R U . . .
H10B H 0.466991 0.244696 0.042163 0.056 Uiso 1 1 calc R U . . .
H10C H 0.592657 0.169200 0.029591 0.056 Uiso 1 1 calc R U . . .


_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
I1B Mo1B 2.8446(4) . ?
I1A Mo1A 2.8524(4) . ?
Mo1A As1A 2.5717(6) . ?
Mo1A C14A 2.258(4) . ?
Mo1A C13A 2.289(4) . ?
Mo1A C2A 1.988(5) . ?
Mo1A C15A 2.312(4) . ?
Mo1A C16A 2.394(4) . ?
Mo1A C12A 2.375(4) . ?
Mo1A C1A 1.967(5) . ?
Mo1B As1B 2.5640(6) . ?
Mo1B C12B 2.371(4) . ?
Mo1B C16B 2.393(5) . ?
Mo1B C15B 2.317(5) . ?
Mo1B C2B 1.976(5) . ?
Mo1B C1B 1.976(5) . ?
Mo1B C13B 2.293(4) . ?
Mo1B C14B 2.273(4) . ?
As1A C6A 1.925(4) . ?
As1A C3A 1.932(5) . ?
As1A C7A 1.946(5) . ?
As1B C6B 1.925(5) . ?
As1B C7B 1.951(4) . ?
As1B C3B 1.933(5) . ?
O1A C1A 1.096(6) . ?
O1B C1B 1.100(6) . ?
O2A C2A 1.139(6) . ?
O2B C2B 1.149(6) . ?
C5A C6A 1.344(6) . ?
C5A C4A 1.493(6) . ?
C5A C10A 1.503(6) . ?
C6A C11A 1.485(6) . ?
C3A C4A 1.342(6) . ?
C3A C8A 1.490(6) . ?
C4A C9A 1.505(6) . ?
C6B C5B 1.352(7) . ?
C6B C11B 1.493(7) . ?
C7B H7BA 0.9600 . ?
C7B H7BB 0.9600 . ?
C7B H7BC 0.9600 . ?
C5B C4B 1.500(7) . ?
C5B C10B 1.492(6) . ?
C12B H12B 0.9300 . ?
C12B C16B 1.410(7) . ?
C12B C13B 1.419(7) . ?
C14A H14A 0.9300 . ?
C14A C13A 1.415(7) . ?
C14A C15A 1.429(7) . ?
C16B H16B 0.9300 . ?
C16B C15B 1.426(7) . ?
C10A H10D 0.9600 . ?
C10A H10E 0.9600 . ?
C10A H10F 0.9600 . ?
C8B H8BA 0.9600 . ?
C8B H8BB 0.9600 . ?
C8B H8BC 0.9600 . ?
C8B C3B 1.479(7) . ?
C15B H15B 0.9300 . ?
C15B C14B 1.419(8) . ?
C13A H13A 0.9300 . ?
C13A C12A 1.426(8) . ?
C15A H15A 0.9300 . ?
C15A C16A 1.406(7) . ?
C16A H16A 0.9300 . ?
C16A C12A 1.409(7) . ?
C3B C4B 1.349(6) . ?
C12A H12A 0.9300 . ?
C7A H7AA 0.9600 . ?
C7A H7AB 0.9600 . ?
C7A H7AC 0.9600 . ?
C4B C9B 1.502(6) . ?
C11A H11D 0.9600 . ?
C11A H11E 0.9600 . ?
C11A H11F 0.9600 . ?
C8A H8AA 0.9600 . ?
C8A H8AB 0.9600 . ?
C8A H8AC 0.9600 . ?
C11B H11A 0.9600 . ?
C11B H11B 0.9600 . ?
C11B H11C 0.9600 . ?
C9A H9AA 0.9600 . ?
C9A H9AB 0.9600 . ?
C9A H9AC 0.9600 . ?
C9B H9BA 0.9600 . ?
C9B H9BB 0.9600 . ?
C9B H9BC 0.9600 . ?
C13B H13B 0.9300 . ?
C13B C14B 1.417(7) . ?
C14B H14B 0.9300 . ?
C10B H10A 0.9600 . ?
C10B H10B 0.9600 . ?
C10B H10C 0.9600 . ?

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
As1A Mo1A I1A 79.360(15) . . ?
C14A Mo1A I1A 136.84(14) . . ?
C14A Mo1A As1A 134.22(13) . . ?
C14A Mo1A C13A 36.25(17) . . ?
C14A Mo1A C15A 36.41(17) . . ?
C14A Mo1A C16A 59.02(18) . . ?
C14A Mo1A C12A 59.50(18) . . ?
C13A Mo1A I1A 140.57(15) . . ?
C13A Mo1A As1A 98.73(13) . . ?
C13A Mo1A C15A 59.73(17) . . ?
C13A Mo1A C16A 58.44(19) . . ?
C13A Mo1A C12A 35.54(19) . . ?
C2A Mo1A I1A 77.18(12) . . ?
C2A Mo1A As1A 121.47(14) . . ?
C2A Mo1A C14A 97.42(18) . . ?
C2A Mo1A C13A 131.85(19) . . ?
C2A Mo1A C15A 91.16(18) . . ?
C2A Mo1A C16A 118.23(19) . . ?
C2A Mo1A C12A 149.53(19) . . ?
C15A Mo1A I1A 100.46(12) . . ?
C15A Mo1A As1A 145.82(13) . . ?
C15A Mo1A C16A 34.71(18) . . ?
C15A Mo1A C12A 58.39(17) . . ?
C16A Mo1A I1A 85.55(12) . . ?
C16A Mo1A As1A 112.34(13) . . ?
C12A Mo1A I1A 105.30(14) . . ?
C12A Mo1A As1A 88.39(13) . . ?
C12A Mo1A C16A 34.35(18) . . ?
C1A Mo1A I1A 128.95(13) . . ?
C1A Mo1A As1A 77.15(14) . . ?
C1A Mo1A C14A 89.98(19) . . ?
C1A Mo1A C13A 87.7(2) . . ?
C1A Mo1A C2A 77.67(19) . . ?
C1A Mo1A C15A 123.73(19) . . ?
C1A Mo1A C16A 145.43(17) . . ?
C1A Mo1A C12A 118.53(19) . . ?
As1B Mo1B I1B 78.735(14) . . ?
C12B Mo1B I1B 103.98(13) . . ?
C12B Mo1B As1B 89.39(12) . . ?
C12B Mo1B C16B 34.43(17) . . ?
C16B Mo1B I1B 83.70(12) . . ?
C16B Mo1B As1B 112.56(13) . . ?
C15B Mo1B I1B 99.29(14) . . ?
C15B Mo1B As1B 146.73(13) . . ?
C15B Mo1B C12B 58.53(17) . . ?
C15B Mo1B C16B 35.20(18) . . ?
C2B Mo1B I1B 78.54(13) . . ?
C2B Mo1B As1B 119.32(13) . . ?
C2B Mo1B C12B 150.77(18) . . ?
C2B Mo1B C16B 119.72(18) . . ?
C2B Mo1B C15B 92.25(18) . . ?
C2B Mo1B C13B 132.20(19) . . ?
C2B Mo1B C14B 98.27(18) . . ?
C1B Mo1B I1B 130.25(14) . . ?
C1B Mo1B As1B 75.93(14) . . ?
C1B Mo1B C12B 117.69(19) . . ?
C1B Mo1B C16B 145.75(18) . . ?
C1B Mo1B C15B 124.7(2) . . ?
C1B Mo1B C2B 77.76(19) . . ?
C1B Mo1B C13B 87.55(19) . . ?
C1B Mo1B C14B 91.1(2) . . ?
C13B Mo1B I1B 139.02(14) . . ?
C13B Mo1B As1B 100.03(14) . . ?
C13B Mo1B C12B 35.38(18) . . ?
C13B Mo1B C16B 58.62(18) . . ?
C13B Mo1B C15B 59.75(18) . . ?
C14B Mo1B I1B 135.30(14) . . ?
C14B Mo1B As1B 135.53(14) . . ?
C14B Mo1B C12B 59.08(18) . . ?
C14B Mo1B C16B 58.96(18) . . ?
C14B Mo1B C15B 36.01(19) . . ?
C14B Mo1B C13B 36.15(19) . . ?
C6A As1A Mo1A 119.11(13) . . ?
C6A As1A C3A 89.20(19) . . ?
C6A As1A C7A 104.72(19) . . ?
C3A As1A Mo1A 120.60(15) . . ?
C3A As1A C7A 105.7(2) . . ?
C7A As1A Mo1A 114.02(14) . . ?
C6B As1B Mo1B 122.12(14) . . ?
C6B As1B C7B 102.8(2) . . ?
C6B As1B C3B 89.7(2) . . ?
C7B As1B Mo1B 112.39(14) . . ?
C3B As1B Mo1B 122.29(14) . . ?
C3B As1B C7B 103.7(2) . . ?
C6A C5A C4A 116.8(4) . . ?
C6A C5A C10A 124.3(4) . . ?
C4A C5A C10A 119.0(4) . . ?
C5A C6A As1A 108.5(3) . . ?
C5A C6A C11A 130.0(4) . . ?
C11A C6A As1A 121.5(3) . . ?
C4A C3A As1A 108.2(3) . . ?
C4A C3A C8A 129.6(4) . . ?
C8A C3A As1A 122.0(3) . . ?
C5A C4A C9A 119.2(4) . . ?
C3A C4A C5A 117.1(4) . . ?
C3A C4A C9A 123.7(4) . . ?
C5B C6B As1B 108.6(4) . . ?
C5B C6B C11B 129.3(4) . . ?
C11B C6B As1B 122.0(3) . . ?
As1B C7B H7BA 109.5 . . ?
As1B C7B H7BB 109.5 . . ?
As1B C7B H7BC 109.5 . . ?
H7BA C7B H7BB 109.5 . . ?
H7BA C7B H7BC 109.5 . . ?
H7BB C7B H7BC 109.5 . . ?
C6B C5B C4B 116.3(4) . . ?
C6B C5B C10B 124.2(5) . . ?
C10B C5B C4B 119.5(5) . . ?
Mo1B C12B H12B 122.9 . . ?
C16B C12B Mo1B 73.6(3) . . ?
C16B C12B H12B 125.8 . . ?
C16B C12B C13B 108.5(4) . . ?
C13B C12B Mo1B 69.3(3) . . ?
C13B C12B H12B 125.8 . . ?
Mo1A C14A H14A 118.8 . . ?
C13A C14A Mo1A 73.1(3) . . ?
C13A C14A H14A 126.3 . . ?
C13A C14A C15A 107.4(5) . . ?
C15A C14A Mo1A 73.8(2) . . ?
C15A C14A H14A 126.3 . . ?
Mo1B C16B H16B 124.1 . . ?
C12B C16B Mo1B 71.9(3) . . ?
C12B C16B H16B 126.1 . . ?
C12B C16B C15B 107.8(5) . . ?
C15B C16B Mo1B 69.5(3) . . ?
C15B C16B H16B 126.1 . . ?
C5A C10A H10D 109.5 . . ?
C5A C10A H10E 109.5 . . ?
C5A C10A H10F 109.5 . . ?
H10D C10A H10E 109.5 . . ?
H10D C10A H10F 109.5 . . ?
H10E C10A H10F 109.5 . . ?
H8BA C8B H8BB 109.5 . . ?
H8BA C8B H8BC 109.5 . . ?
H8BB C8B H8BC 109.5 . . ?
C3B C8B H8BA 109.5 . . ?
C3B C8B H8BB 109.5 . . ?
C3B C8B H8BC 109.5 . . ?
Mo1B C15B H15B 120.1 . . ?
C16B C15B Mo1B 75.3(3) . . ?
C16B C15B H15B 126.1 . . ?
C14B C15B Mo1B 70.3(3) . . ?
C14B C15B C16B 107.8(4) . . ?
C14B C15B H15B 126.1 . . ?
Mo1A C13A H13A 119.7 . . ?
C14A C13A Mo1A 70.7(2) . . ?
C14A C13A H13A 125.9 . . ?
C14A C13A C12A 108.2(5) . . ?
C12A C13A Mo1A 75.5(3) . . ?
C12A C13A H13A 125.9 . . ?
O2B C2B Mo1B 177.3(4) . . ?
O2A C2A Mo1A 177.3(4) . . ?
Mo1A C15A H15A 120.2 . . ?
C14A C15A Mo1A 69.8(3) . . ?
C14A C15A H15A 125.9 . . ?
C16A C15A Mo1A 75.9(3) . . ?
C16A C15A C14A 108.1(4) . . ?
C16A C15A H15A 125.9 . . ?
Mo1A C16A H16A 124.4 . . ?
C15A C16A Mo1A 69.4(3) . . ?
C15A C16A H16A 125.7 . . ?
C15A C16A C12A 108.7(5) . . ?
C12A C16A Mo1A 72.1(3) . . ?
C12A C16A H16A 125.7 . . ?
C8B C3B As1B 121.7(3) . . ?
C4B C3B As1B 107.8(4) . . ?
C4B C3B C8B 130.4(4) . . ?
Mo1A C12A H12A 122.9 . . ?
C13A C12A Mo1A 68.9(3) . . ?
C13A C12A H12A 126.2 . . ?
C16A C12A Mo1A 73.6(3) . . ?
C16A C12A C13A 107.7(4) . . ?
C16A C12A H12A 126.2 . . ?
As1A C7A H7AA 109.5 . . ?
As1A C7A H7AB 109.5 . . ?
As1A C7A H7AC 109.5 . . ?
H7AA C7A H7AB 109.5 . . ?
H7AA C7A H7AC 109.5 . . ?
H7AB C7A H7AC 109.5 . . ?
C5B C4B C9B 119.1(4) . . ?
C3B C4B C5B 117.4(4) . . ?
C3B C4B C9B 123.4(5) . . ?
C6A C11A H11D 109.5 . . ?
C6A C11A H11E 109.5 . . ?
C6A C11A H11F 109.5 . . ?
H11D C11A H11E 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?
C3A C8A H8AA 109.5 . . ?
C3A C8A H8AB 109.5 . . ?
C3A C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C6B C11B H11A 109.5 . . ?
C6B C11B H11B 109.5 . . ?
C6B C11B H11C 109.5 . . ?
H11A C11B H11B 109.5 . . ?
H11A C11B H11C 109.5 . . ?
H11B C11B H11C 109.5 . . ?
O1A C1A Mo1A 178.4(4) . . ?
C4A C9A H9AA 109.5 . . ?
C4A C9A H9AB 109.5 . . ?
C4A C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
O1B C1B Mo1B 176.3(4) . . ?
C4B C9B H9BA 109.5 . . ?
C4B C9B H9BB 109.5 . . ?
C4B C9B H9BC 109.5 . . ?
H9BA C9B H9BB 109.5 . . ?
H9BA C9B H9BC 109.5 . . ?
H9BB C9B H9BC 109.5 . . ?
Mo1B C13B H13B 119.3 . . ?
C12B C13B Mo1B 75.3(3) . . ?
C12B C13B H13B 126.1 . . ?
C14B C13B Mo1B 71.2(2) . . ?
C14B C13B C12B 107.8(5) . . ?
C14B C13B H13B 126.1 . . ?
Mo1B C14B H14B 119.5 . . ?
C15B C14B Mo1B 73.7(3) . . ?
C15B C14B H14B 125.9 . . ?
C13B C14B Mo1B 72.7(3) . . ?
C13B C14B C15B 108.1(5) . . ?
C13B C14B H14B 125.9 . . ?
C5B C10B H10A 109.5 . . ?
C5B C10B H10B 109.5 . . ?
C5B C10B H10C 109.5 . . ?
H10A C10B H10B 109.5 . . ?
H10A C10B H10C 109.5 . . ?
H10B C10B H10C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1A C14A C13A C12A 66.8(3) . . . . ?
Mo1A C14A C15A C16A -66.8(3) . . . . ?
Mo1A C13A C12A C16A 63.9(3) . . . . ?
Mo1A C15A C16A C12A -61.7(3) . . . . ?
Mo1A C16A C12A C13A -60.9(3) . . . . ?
Mo1B C12B C16B C15B -60.5(3) . . . . ?
Mo1B C12B C13B C14B 64.3(3) . . . . ?
Mo1B C16B C15B C14B -63.3(3) . . . . ?
Mo1B C15B C14B C13B -65.0(3) . . . . ?
Mo1B C13B C14B C15B 65.7(3) . . . . ?
As1A C3A C4A C5A -4.1(5) . . . . ?
As1A C3A C4A C9A 176.1(4) . . . . ?
As1B C6B C5B C4B -0.3(5) . . . . ?
As1B C6B C5B C10B -179.4(4) . . . . ?
As1B C3B C4B C5B 2.3(5) . . . . ?
As1B C3B C4B C9B -178.8(4) . . . . ?
C6A C5A C4A C3A -0.1(6) . . . . ?
C6A C5A C4A C9A 179.7(4) . . . . ?
C4A C5A C6A As1A 4.3(5) . . . . ?
C4A C5A C6A C11A -175.8(4) . . . . ?
C6B C5B C4B C3B -1.4(6) . . . . ?
C6B C5B C4B C9B 179.6(4) . . . . ?
C12B C16B C15B Mo1B 62.1(3) . . . . ?
C12B C16B C15B C14B -1.2(5) . . . . ?
C12B C13B C14B Mo1B -67.0(3) . . . . ?
C12B C13B C14B C15B -1.3(5) . . . . ?
C14A C13A C12A Mo1A -63.6(3) . . . . ?
C14A C13A C12A C16A 0.3(5) . . . . ?
C14A C15A C16A Mo1A 62.8(3) . . . . ?
C14A C15A C16A C12A 1.1(5) . . . . ?
C16B C12B C13B Mo1B -63.7(3) . . . . ?
C16B C12B C13B C14B 0.6(5) . . . . ?
C16B C15B C14B Mo1B 66.6(3) . . . . ?
C16B C15B C14B C13B 1.5(5) . . . . ?
C10A C5A C6A As1A -177.0(4) . . . . ?
C10A C5A C6A C11A 2.9(8) . . . . ?
C10A C5A C4A C3A -178.9(4) . . . . ?
C10A C5A C4A C9A 0.9(7) . . . . ?
C8B C3B C4B C5B 179.4(4) . . . . ?
C8B C3B C4B C9B -1.7(8) . . . . ?
C13A C14A C15A Mo1A 65.9(3) . . . . ?
C13A C14A C15A C16A -0.9(5) . . . . ?
C15A C14A C13A Mo1A -66.4(3) . . . . ?
C15A C14A C13A C12A 0.4(5) . . . . ?
C15A C16A C12A Mo1A 60.1(3) . . . . ?
C15A C16A C12A C13A -0.8(5) . . . . ?
C8A C3A C4A C5A -177.9(5) . . . . ?
C8A C3A C4A C9A 2.3(9) . . . . ?
C11B C6B C5B C4B 177.5(4) . . . . ?
C11B C6B C5B C10B -1.7(8) . . . . ?
C13B C12B C16B Mo1B 60.9(3) . . . . ?
C13B C12B C16B C15B 0.4(5) . . . . ?
C10B C5B C4B C3B 177.8(4) . . . . ?
C10B C5B C4B C9B -1.2(6) . . . . ?


_ins_header                      
;
TITL RMK_219_C_red_a_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   8.857208  13.920570  16.071542 104.8674 104.3165  91.7418
ZERR    5.00   0.000296   0.000398   0.000527   0.0027   0.0029   0.0025
LATT  1
SFAC C H O As Mo I
UNIT 80.00 100.00 15.00 5.00 5.00 5.00
TREF
HKLF 4
END
;
_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 1.435
_oxdiff_exptl_absorpt_empirical_full_min 0.713
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-hexane'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_rmk_211_c_scale
_database_code_depnum_ccdc_archive 'CCDC 2149526'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2022-02-01 deposited with the CCDC.	2024-06-27 downloaded from the CCDC.
;
_audit_creation_date             2022-02-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H22.998 As'
_chemical_formula_sum            'C29 H23 As'
_chemical_formula_weight         446.39
_chemical_melting_point          ?
_chemical_oxdiff_formula         C29H23As
_chemical_oxdiff_usercomment     'DCM/MeOH at -20'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
As As -0.9300 1.0051 '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           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   26.5014(2)
_cell_length_b                   26.5014(2)
_cell_length_c                   12.16700(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8545.18(15)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    6296
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.3400
_cell_measurement_theta_min      5.1920
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3680
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
8 15 0 0.0691
6 10 -6 0.0723
-5 -9 -6 0.0591
-8 -15 0 0.0716
7 12 5 0.0877
-4 -8 7 0.0844
-15 8 -1 0.0425
15 -8 1 0.0406
-6 16 0 0.0552
-15 1 4 0.0552

_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.083
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
8.3884 15.0168 -0.0053 0.3453 0.5614 -0.7520
5.5194 9.8153 -5.9682 -0.0691 -0.1175 -0.9907
-4.9534 -8.9373 -6.3516 -0.5196 -0.8503 -0.0842
-8.3810 -15.0069 -0.2976 -0.3600 -0.5857 0.7262
6.5382 11.7587 4.9196 0.5137 0.8395 -0.1769
-4.4441 -7.8821 6.7146 0.1505 0.2504 0.9564
-14.8580 8.3314 -1.1188 -0.8988 0.4278 -0.0956
14.8275 -8.3727 1.1389 0.8985 -0.4276 0.0995
-5.6407 16.2531 -0.0844 -0.4109 0.7573 -0.5076
-15.3225 0.8297 3.5745 -0.6403 0.4885 0.5928

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0137
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11604
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.569
_diffrn_reflns_theta_min         3.998
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     44.00  69.00   1.00    5.00    --   36.95 -99.00-120.00   25
  2  ω     31.00  85.00   1.00    5.00    --   36.95-125.00  60.00   54
  3  ω    -32.00  48.00   1.00    5.00    --   36.95 -38.00-180.00   80
  4  ω     41.00  69.00   1.00   25.00    --  111.00-111.00 150.00   28
  5  ω    140.00 174.00   1.00   25.00    --  111.00  38.00  60.00   34
  6  ω     45.00  70.00   1.00   25.00    --  111.00 -64.00-120.00   25
  7  ω    144.00 172.00   1.00   25.00    --  111.00 111.00-150.00   28
  8  ω    106.00 131.00   1.00   25.00    --  111.00 111.00-150.00   25
  9  ω     98.00 131.00   1.00   25.00    --  111.00 -64.00-120.00   33
 10  ω     93.00 133.00   1.00   25.00    --  111.00  38.00  60.00   40
 11  ω     55.00  90.00   1.00   25.00    --  111.00 -92.00-150.00   35
 12  ω     45.00  78.00   1.00   25.00    --  111.00 -92.00-180.00   33
 13  ω     46.00  72.00   1.00   25.00    --  111.00 -77.00 -60.00   26
 14  ω     90.00 121.00   1.00   25.00    --  111.00 -77.00 -60.00   31
 15  ω    131.00 177.00   1.00   25.00    --  111.00  77.00 -60.00   46
 16  ω    139.00 172.00   1.00   25.00    --  111.00  77.00 -90.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0530373000
_diffrn_orient_matrix_UB_12      -0.0066150000
_diffrn_orient_matrix_UB_13      0.0497497000
_diffrn_orient_matrix_UB_21      -0.0106024000
_diffrn_orient_matrix_UB_22      0.0433386000
_diffrn_orient_matrix_UB_23      0.0811535000
_diffrn_orient_matrix_UB_31      -0.0212619000
_diffrn_orient_matrix_UB_32      -0.0381732000
_diffrn_orient_matrix_UB_33      0.0835479000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4103
_reflns_number_total             4256
_reflns_odcompleteness_completeness 97.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4256
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0399
_refine_ls_restrained_S_all      1.183
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0372P)²+19.0023P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1001
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 As1-C5 \\sim As1'-C5
 with sigma of 0.02
 As1-C1 \\sim As1'-C1'
 with sigma of 0.02
 C1-H1A \\sim C1'-H1A
 with sigma of 0.02
 As1-C2 \\sim As1'-C2
 with sigma of 0.02
 C1-H1B \\sim C1'-H1B
 with sigma of 0.02
 C1-H1C \\sim C1'-H1C
 with sigma of 0.02
 As1-H1A \\sim As1'-H1A
 with sigma of 0.04
 As1-H1B \\sim As1'-H1B
 with sigma of 0.04
 As1-H1C \\sim As1'-H1C
 with sigma of 0.04
 C5-C1 \\sim C5-C1'
 with sigma of 0.04
 C1-C2 \\sim C1'-C2
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C1') = Uanis(C1)
4. Others
 Sof(As1')=Sof(C1')=Sof(H1'A)=Sof(H1'B)=Sof(H1'C)=1-FVAR(1)
 Sof(As1)=Sof(C1)=FVAR(1)
 Fixed Sof: H1A(0.88921) H1B(0.88921) H1C(0.88921)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C25(H25), C23(H23), C29(H29), C19(H19), C15(H15), C17(H17), C9(H9),
 C27(H27), C26(H26), C14(H14), C16(H16), C11(H11), C10(H10), C13(H13), C22(H22),
  C8(H8), C20(H20), C28(H28), C21(H21)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1'(H1'A,H1'B,H1'C)
;
_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
As1 As 0.74422(2) 0.75981(2) 0.57838(3) 0.02590(12) Uani 0.8899(15) 1 d D . P A
1
C24 C 0.64919(9) 0.70777(9) 0.6477(2) 0.0278(5) Uani 1 1 d . . . . .
C4 C 0.70745(8) 0.66961(8) 0.5028(2) 0.0268(5) Uani 1 1 d . . . . .
C6 C 0.82095(9) 0.74487(8) 0.3991(2) 0.0292(5) Uani 1 1 d . . . . .
C7 C 0.86221(9) 0.76464(9) 0.4549(2) 0.0340(5) Uani 1 1 d . . . . .
H7 H 0.862254 0.764362 0.531357 0.041 Uiso 1 1 calc R U . . .
C5 C 0.69221(9) 0.70772(8) 0.5707(2) 0.0290(5) Uani 1 1 d D . . . .
C18 C 0.67938(9) 0.62122(9) 0.49249(19) 0.0281(5) Uani 1 1 d . . . . .
C25 C 0.64004(9) 0.66786(9) 0.7204(2) 0.0322(5) Uani 1 1 d . . . . .
H25 H 0.660935 0.639666 0.718874 0.039 Uiso 1 1 calc R U . . .
C3 C 0.75422(8) 0.67875(9) 0.4392(2) 0.0278(5) Uani 1 1 d . . . . .
C23 C 0.62820(9) 0.62089(10) 0.4666(2) 0.0331(5) Uani 1 1 d . . . . .
H23 H 0.611490 0.651293 0.455007 0.040 Uiso 1 1 calc R U . . .
C12 C 0.77584(9) 0.64034(8) 0.3635(2) 0.0277(5) Uani 1 1 d . . . . .
C29 C 0.61691(10) 0.74903(10) 0.6524(2) 0.0352(5) Uani 1 1 d . . . . .
H29 H 0.622512 0.776378 0.606116 0.042 Uiso 1 1 calc R U . . .
C19 C 0.70386(10) 0.57509(9) 0.5083(2) 0.0329(5) Uani 1 1 d . . . . .
H19 H 0.738189 0.574398 0.524133 0.040 Uiso 1 1 calc R U . . .
C1 C 0.71562(11) 0.81679(10) 0.4947(2) 0.0334(6) Uani 0.8899(15) 1 d D . P A 1
H1A H 0.695939 0.804061 0.434502 0.050 Uiso 0.8892 1 calc R U P A 1
H1B H 0.742505 0.837409 0.466717 0.050 Uiso 0.8892 1 calc R U P A 1
H1C H 0.694507 0.836635 0.542009 0.050 Uiso 0.8892 1 calc R U P A 1
C15 C 0.82003(11) 0.56951(10) 0.2224(2) 0.0418(6) Uani 1 1 d . . . . .
H15 H 0.834810 0.546271 0.175046 0.050 Uiso 1 1 calc R U . . .
C17 C 0.74731(10) 0.61749(9) 0.2806(2) 0.0337(5) Uani 1 1 d . . . . .
H17 H 0.713491 0.625970 0.271924 0.040 Uiso 1 1 calc R U . . .
C9 C 0.90412(10) 0.78581(10) 0.2858(3) 0.0403(6) Uani 1 1 d . . . . .
H9 H 0.931600 0.799300 0.248485 0.048 Uiso 1 1 calc R U . . .
C2 C 0.77679(9) 0.72391(9) 0.4572(2) 0.0298(5) Uani 1 1 d D . . . .
C27 C 0.56786(10) 0.71090(11) 0.7966(2) 0.0377(6) Uani 1 1 d . . . . .
H27 H 0.540850 0.711901 0.845335 0.045 Uiso 1 1 calc R U . . .
C26 C 0.60022(10) 0.66965(10) 0.7948(2) 0.0354(5) Uani 1 1 d . . . . .
H26 H 0.595238 0.643106 0.843608 0.042 Uiso 1 1 calc R U . . .
C14 C 0.84826(10) 0.59186(10) 0.3049(2) 0.0387(6) Uani 1 1 d . . . . .
H14 H 0.882083 0.583330 0.313267 0.046 Uiso 1 1 calc R U . . .
C16 C 0.76932(11) 0.58217(10) 0.2111(2) 0.0410(6) Uani 1 1 d . . . . .
H16 H 0.750027 0.566863 0.156683 0.049 Uiso 1 1 calc R U . . .
C11 C 0.82242(9) 0.74607(10) 0.2838(2) 0.0353(5) Uani 1 1 d . . . . .
H11 H 0.795510 0.732992 0.243832 0.042 Uiso 1 1 calc R U . . .
C10 C 0.86324(11) 0.76638(10) 0.2288(2) 0.0400(6) Uani 1 1 d . . . . .
H10 H 0.863297 0.767023 0.152409 0.048 Uiso 1 1 calc R U . . .
C13 C 0.82663(9) 0.62661(9) 0.3746(2) 0.0324(5) Uani 1 1 d . . . . .
H13 H 0.846021 0.641180 0.429875 0.039 Uiso 1 1 calc R U . . .
C22 C 0.60187(11) 0.57607(11) 0.4578(2) 0.0428(6) Uani 1 1 d . . . . .
H22 H 0.567779 0.576447 0.439699 0.051 Uiso 1 1 calc R U . . .
C8 C 0.90320(10) 0.78472(10) 0.3999(3) 0.0405(6) Uani 1 1 d . . . . .
H8 H 0.930324 0.797564 0.439469 0.049 Uiso 1 1 calc R U . . .
C20 C 0.67695(12) 0.53031(10) 0.5005(2) 0.0416(6) Uani 1 1 d . . . . .
H20 H 0.693282 0.499688 0.511852 0.050 Uiso 1 1 calc R U . . .
C28 C 0.57640(10) 0.75029(11) 0.7250(2) 0.0404(6) Uani 1 1 d . . . . .
H28 H 0.554853 0.777985 0.725305 0.048 Uiso 1 1 calc R U . . .
C21 C 0.62604(12) 0.53092(11) 0.4759(3) 0.0472(7) Uani 1 1 d . . . . .
H21 H 0.608134 0.500806 0.471616 0.057 Uiso 1 1 calc R U . . .
As1' As 0.72868(11) 0.76971(10) 0.5067(3) 0.0384(11) Uani 0.1101(15) 1 d D . P
A 2
C1' C 0.7669(8) 0.7852(8) 0.6446(15) 0.0334(6) Uani 0.1101(15) 1 d D . P A 2
H1'A H 0.744777 0.782096 0.706764 0.050 Uiso 0.1101(15) 1 calc R U P A 2
H1'B H 0.779738 0.819074 0.641072 0.050 Uiso 0.1101(15) 1 calc R U P A 2
H1'C H 0.794462 0.762010 0.652213 0.050 Uiso 0.1101(15) 1 calc R U P A 2


_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
As1 C5 1.953(2) . ?
As1 C1 1.973(3) . ?
As1 C2 1.955(3) . ?
C24 C5 1.476(3) . ?
C24 C25 1.400(3) . ?
C24 C29 1.390(3) . ?
C4 C5 1.366(3) . ?
C4 C18 1.488(3) . ?
C4 C3 1.481(3) . ?
C6 C7 1.390(3) . ?
C6 C2 1.476(3) . ?
C6 C11 1.403(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.383(4) . ?
C5 As1' 2.059(4) . ?
C18 C23 1.393(3) . ?
C18 C19 1.397(3) . ?
C25 H25 0.9300 . ?
C25 C26 1.392(4) . ?
C3 C12 1.487(3) . ?
C3 C2 1.356(3) . ?
C23 H23 0.9300 . ?
C23 C22 1.382(4) . ?
C12 C17 1.398(3) . ?
C12 C13 1.401(3) . ?
C29 H29 0.9300 . ?
C29 C28 1.391(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.388(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C15 H15 0.9300 . ?
C15 C14 1.385(4) . ?
C15 C16 1.392(4) . ?
C17 H17 0.9300 . ?
C17 C16 1.390(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.386(4) . ?
C9 C8 1.388(4) . ?
C2 As1' 1.860(4) . ?
C27 H27 0.9300 . ?
C27 C26 1.389(4) . ?
C27 C28 1.378(4) . ?
C26 H26 0.9300 . ?
C14 H14 0.9300 . ?
C14 C13 1.377(4) . ?
C16 H16 0.9300 . ?
C11 H11 0.9300 . ?
C11 C10 1.381(4) . ?
C10 H10 0.9300 . ?
C13 H13 0.9300 . ?
C22 H22 0.9300 . ?
C22 C21 1.375(5) . ?
C8 H8 0.9300 . ?
C20 H20 0.9300 . ?
C20 C21 1.382(5) . ?
C28 H28 0.9300 . ?
C21 H21 0.9300 . ?
As1' C1' 2.003(15) . ?
C1' H1'A 0.9600 . ?
C1' H1'B 0.9600 . ?
C1' H1'C 0.9600 . ?

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
C5 As1 C1 104.18(11) . . ?
C5 As1 C2 86.07(10) . . ?
C2 As1 C1 98.79(11) . . ?
C25 C24 C5 122.3(2) . . ?
C29 C24 C5 120.2(2) . . ?
C29 C24 C25 117.5(2) . . ?
C5 C4 C18 122.7(2) . . ?
C5 C4 C3 116.3(2) . . ?
C3 C4 C18 121.0(2) . . ?
C7 C6 C2 122.1(2) . . ?
C7 C6 C11 117.3(2) . . ?
C11 C6 C2 120.6(2) . . ?
C6 C7 H7 119.1 . . ?
C8 C7 C6 121.7(3) . . ?
C8 C7 H7 119.1 . . ?
C24 C5 As1 120.95(17) . . ?
C24 C5 As1' 127.03(18) . . ?
C4 C5 As1 110.06(17) . . ?
C4 C5 C24 127.8(2) . . ?
C4 C5 As1' 102.86(19) . . ?
C23 C18 C4 120.8(2) . . ?
C23 C18 C19 118.6(2) . . ?
C19 C18 C4 120.7(2) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 C24 121.1(2) . . ?
C26 C25 H25 119.4 . . ?
C4 C3 C12 122.3(2) . . ?
C2 C3 C4 115.4(2) . . ?
C2 C3 C12 122.3(2) . . ?
C18 C23 H23 119.5 . . ?
C22 C23 C18 121.0(3) . . ?
C22 C23 H23 119.5 . . ?
C17 C12 C3 122.3(2) . . ?
C17 C12 C13 118.5(2) . . ?
C13 C12 C3 119.2(2) . . ?
C24 C29 H29 119.3 . . ?
C24 C29 C28 121.4(2) . . ?
C28 C29 H29 119.3 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 120.0(3) . . ?
C20 C19 H19 120.0 . . ?
As1 C1 H1A 109.5 . . ?
As1 C1 H1B 109.5 . . ?
As1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C14 C15 H15 120.3 . . ?
C14 C15 C16 119.3(3) . . ?
C16 C15 H15 120.3 . . ?
C12 C17 H17 119.9 . . ?
C16 C17 C12 120.2(2) . . ?
C16 C17 H17 119.9 . . ?
C10 C9 H9 120.7 . . ?
C10 C9 C8 118.6(3) . . ?
C8 C9 H9 120.7 . . ?
C6 C2 As1 121.88(17) . . ?
C6 C2 As1' 116.92(18) . . ?
C3 C2 As1 110.90(18) . . ?
C3 C2 C6 127.2(2) . . ?
C3 C2 As1' 109.02(19) . . ?
C26 C27 H27 120.5 . . ?
C28 C27 H27 120.5 . . ?
C28 C27 C26 119.0(3) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 C25 120.3(2) . . ?
C27 C26 H26 119.8 . . ?
C15 C14 H14 119.7 . . ?
C13 C14 C15 120.5(3) . . ?
C13 C14 H14 119.7 . . ?
C15 C16 H16 119.7 . . ?
C17 C16 C15 120.5(3) . . ?
C17 C16 H16 119.7 . . ?
C6 C11 H11 119.5 . . ?
C10 C11 C6 121.0(2) . . ?
C10 C11 H11 119.5 . . ?
C9 C10 H10 119.5 . . ?
C11 C10 C9 121.0(3) . . ?
C11 C10 H10 119.5 . . ?
C12 C13 H13 119.5 . . ?
C14 C13 C12 120.9(2) . . ?
C14 C13 H13 119.5 . . ?
C23 C22 H22 120.0 . . ?
C21 C22 C23 120.0(3) . . ?
C21 C22 H22 120.0 . . ?
C7 C8 C9 120.4(3) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C19 C20 H20 119.8 . . ?
C21 C20 C19 120.4(3) . . ?
C21 C20 H20 119.8 . . ?
C29 C28 H28 119.7 . . ?
C27 C28 C29 120.7(2) . . ?
C27 C28 H28 119.7 . . ?
C22 C21 C20 120.0(2) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C2 As1' C5 85.61(14) . . ?
C2 As1' C1' 93.4(6) . . ?
C1' As1' C5 94.8(6) . . ?
As1' C1' H1'A 109.5 . . ?
As1' C1' H1'B 109.5 . . ?
As1' C1' H1'C 109.5 . . ?
H1'A C1' H1'B 109.5 . . ?
H1'A C1' H1'C 109.5 . . ?
H1'B C1' H1'C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C24 C25 C26 C27 1.5(4) . . . . ?
C24 C29 C28 C27 1.6(4) . . . . ?
C4 C18 C23 C22 -179.4(2) . . . . ?
C4 C18 C19 C20 178.8(2) . . . . ?
C4 C3 C12 C17 52.8(3) . . . . ?
C4 C3 C12 C13 -127.6(2) . . . . ?
C4 C3 C2 As1 7.4(3) . . . . ?
C4 C3 C2 C6 -174.4(2) . . . . ?
C4 C3 C2 As1' -24.8(3) . . . . ?
C6 C7 C8 C9 0.2(4) . . . . ?
C6 C2 As1' C5 -178.0(2) . . . . ?
C6 C2 As1' C1' -83.4(7) . . . . ?
C6 C11 C10 C9 0.5(4) . . . . ?
C7 C6 C2 As1 47.6(3) . . . . ?
C7 C6 C2 C3 -130.4(3) . . . . ?
C7 C6 C2 As1' 82.0(3) . . . . ?
C7 C6 C11 C10 -0.3(4) . . . . ?
C5 C24 C25 C26 177.7(2) . . . . ?
C5 C24 C29 C28 -179.3(2) . . . . ?
C5 C4 C18 C23 54.2(3) . . . . ?
C5 C4 C18 C19 -126.0(3) . . . . ?
C5 C4 C3 C12 178.9(2) . . . . ?
C5 C4 C3 C2 0.9(3) . . . . ?
C18 C4 C5 As1 171.10(18) . . . . ?
C18 C4 C5 C24 3.6(4) . . . . ?
C18 C4 C5 As1' -159.9(2) . . . . ?
C18 C4 C3 C12 -0.8(3) . . . . ?
C18 C4 C3 C2 -178.9(2) . . . . ?
C18 C23 C22 C21 0.7(4) . . . . ?
C18 C19 C20 C21 0.7(4) . . . . ?
C25 C24 C5 As1 -119.0(2) . . . . ?
C25 C24 C5 C4 47.3(4) . . . . ?
C25 C24 C5 As1' -153.0(2) . . . . ?
C25 C24 C29 C28 -1.3(4) . . . . ?
C3 C4 C5 As1 -8.6(3) . . . . ?
C3 C4 C5 C24 -176.1(2) . . . . ?
C3 C4 C5 As1' 20.4(3) . . . . ?
C3 C4 C18 C23 -126.1(3) . . . . ?
C3 C4 C18 C19 53.7(3) . . . . ?
C3 C12 C17 C16 179.3(2) . . . . ?
C3 C12 C13 C14 -178.8(2) . . . . ?
C3 C2 As1' C5 28.9(2) . . . . ?
C3 C2 As1' C1' 123.5(7) . . . . ?
C23 C18 C19 C20 -1.4(4) . . . . ?
C23 C22 C21 C20 -1.4(4) . . . . ?
C12 C3 C2 As1 -170.64(18) . . . . ?
C12 C3 C2 C6 7.5(4) . . . . ?
C12 C3 C2 As1' 157.2(2) . . . . ?
C12 C17 C16 C15 -0.7(4) . . . . ?
C29 C24 C5 As1 59.0(3) . . . . ?
C29 C24 C5 C4 -134.8(3) . . . . ?
C29 C24 C5 As1' 24.9(4) . . . . ?
C29 C24 C25 C26 -0.3(4) . . . . ?
C19 C18 C23 C22 0.7(4) . . . . ?
C19 C20 C21 C22 0.7(4) . . . . ?
C15 C14 C13 C12 -0.3(4) . . . . ?
C17 C12 C13 C14 0.7(4) . . . . ?
C2 C6 C7 C8 -179.3(2) . . . . ?
C2 C6 C11 C10 178.9(2) . . . . ?
C2 C3 C12 C17 -129.2(3) . . . . ?
C2 C3 C12 C13 50.3(3) . . . . ?
C26 C27 C28 C29 -0.3(4) . . . . ?
C14 C15 C16 C17 1.1(4) . . . . ?
C16 C15 C14 C13 -0.6(4) . . . . ?
C11 C6 C7 C8 0.0(4) . . . . ?
C11 C6 C2 As1 -131.7(2) . . . . ?
C11 C6 C2 C3 50.3(4) . . . . ?
C11 C6 C2 As1' -97.2(3) . . . . ?
C10 C9 C8 C7 -0.1(4) . . . . ?
C13 C12 C17 C16 -0.2(4) . . . . ?
C8 C9 C10 C11 -0.3(4) . . . . ?
C28 C27 C26 C25 -1.2(4) . . . . ?


_ins_header                      
;
TITL RMK_211_C_scale in I4(1)/a 
REM I4(1)/a (#88 in standard setting)
CELL 1.54184  26.501388  26.501388  12.166972  90.0000  90.0000  90.0000
ZERR   16.00   0.000199   0.000199   0.000134   0.0000   0.0000   0.0000
LATT  2
SYMM -x+1/2,-y, z+1/2 
SYMM -y+3/4, x+1/4, z+1/4 
SYMM  y+3/4,-x+3/4, z+3/4 
SFAC C H As
UNIT 464.00 368.00 16.00
TREF
HKLF 4
END
;
_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 1.060
_oxdiff_exptl_absorpt_empirical_full_min 0.943
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH2Cl2/n-hexane'
####################################################################### 
# 
# 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_rmk_225_e_scale
_database_code_depnum_ccdc_archive 'CCDC 2145367'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2022-01-29 deposited with the CCDC.	2024-06-27 downloaded from the CCDC.
;
_audit_creation_date             2022-01-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C22 H23 As Mo O7'
_chemical_formula_sum            'C22 H23 As Mo O7'
_chemical_formula_weight         570.26
_chemical_melting_point          ?
_chemical_oxdiff_formula         C22H23As1Mo1O7
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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3557(3)
_cell_length_b                   8.5540(2)
_cell_length_c                   15.9822(6)
_cell_angle_alpha                80.769(3)
_cell_angle_beta                 87.205(3)
_cell_angle_gamma                81.552(2)
_cell_volume                     1114.92(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10561
_cell_measurement_temperature    149.98(15)
_cell_measurement_theta_max      31.9190
_cell_measurement_theta_min      4.2070
_shelx_estimated_absorpt_T_max   0.867
_shelx_estimated_absorpt_T_min   0.475
_exptl_absorpt_coefficient_mu    2.101
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             572
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 -11 -4 0.0779
-2 11 4 0.0779
10 7 9 0.1585
-11 -3 -8 0.1770
0 0 -22 0.0423
0 0 22 0.0194

_exptl_crystal_size_max          0.416
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.07
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.2513 -11.3524 -4.4247 0.0717 0.2993 -0.9515
-2.2513 11.3524 4.4247 -0.0717 -0.2993 0.9515
9.5657 7.3546 9.4646 -0.2331 -0.9715 0.0422
-11.0643 -3.4915 -8.3973 0.2211 0.9214 0.3197
-0.0332 0.0856 -22.2090 0.9956 0.0785 0.0508
-0.2971 0.4914 22.3328 -0.9969 -0.0786 0.0088

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23753
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.639
_diffrn_reflns_theta_min         3.265
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.98(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  42.00   1.00   12.63    --  -17.69  77.00 -30.00   92
  2  ω    -74.00  -6.00   1.00   12.63    --  -17.69 125.00  95.61   68
  3  ω    -10.00  91.00   1.00   12.63    --   18.00  57.00-120.00  101
  4  ω     -6.00  91.00   1.00   12.63    --   18.00  37.00  30.00   97
  5  ω    -41.00  51.00   1.00   12.63    --   18.00 -77.00-120.00   92
  6  ω    -42.00  51.00   1.00   12.63    --   18.00 -77.00  90.00   93
  7  ω     -9.00  90.00   1.00   12.63    --   18.00  57.00 120.00   99
  8  ω    -15.00  19.00   1.00   12.63    --   18.00  77.00   0.00   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0098754000
_diffrn_orient_matrix_UB_12      0.0131010000
_diffrn_orient_matrix_UB_13      -0.0447940000
_diffrn_orient_matrix_UB_21      -0.0683970000
_diffrn_orient_matrix_UB_22      -0.0385314000
_diffrn_orient_matrix_UB_23      -0.0035795000
_diffrn_orient_matrix_UB_31      -0.0509327000
_diffrn_orient_matrix_UB_32      0.0744611000
_diffrn_orient_matrix_UB_33      -0.0019224000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\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                5997
_reflns_number_total             7225
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         7225
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0308
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0240P)²+0.3554P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0678
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C18(H18), C20(H20), C21(H21), C22(H22)
2.b Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C8(H8a,H8b,H8c), C15(H15a,H15b,H15c), C14(H14a,H14b,
 H14c), C16(H16a,H16b,H16c), C9(H9a,H9b,H9c)
;
_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 0.77444(2) 0.75484(2) 0.59767(2) 0.01584(5) Uani 1 1 d . . . . .
As1 As 0.61480(2) 0.84422(2) 0.72297(2) 0.01335(5) Uani 1 1 d . . . . .
O3 O 0.91974(18) 0.43622(18) 0.69897(10) 0.0271(4) Uani 1 1 d . . . . .
O6 O 0.7416(2) 0.8744(2) 0.93228(11) 0.0326(4) Uani 1 1 d . . . . .
O5 O 0.83842(18) 0.35806(18) 0.89427(11) 0.0277(4) Uani 1 1 d . . . . .
O7 O 0.5920(2) 0.6742(2) 0.94908(10) 0.0323(4) Uani 1 1 d . . . . .
O4 O 1.05129(17) 0.49094(18) 0.89250(11) 0.0274(4) Uani 1 1 d . . . . .
O2 O 1.14647(18) 0.7411(2) 0.60898(11) 0.0398(5) Uani 1 1 d . . . . .
C5 C 0.7306(2) 0.7243(2) 0.82071(13) 0.0157(4) Uani 1 1 d . . . . .
O1 O 0.8382(2) 1.1106(2) 0.57110(13) 0.0459(5) Uani 1 1 d . . . . .
C4 C 0.8314(2) 0.5991(2) 0.80121(13) 0.0161(4) Uani 1 1 d . . . . .
C10 C 0.5370(2) 1.0552(2) 0.74807(13) 0.0177(4) Uani 1 1 d . . . . .
C3 C 0.8550(2) 0.5691(2) 0.70896(13) 0.0170(4) Uani 1 1 d . . . . .
C13 C 0.4027(2) 0.7856(2) 0.75113(13) 0.0165(4) Uani 1 1 d . . . . .
C7 C 0.6916(2) 0.7679(2) 0.90617(13) 0.0184(4) Uani 1 1 d . . . . .
C12 C 0.3021(2) 0.9159(2) 0.76564(13) 0.0180(4) Uani 1 1 d . . . . .
C11 C 0.3763(2) 1.0654(2) 0.76234(13) 0.0184(4) Uani 1 1 d . . . . .
C6 C 0.9221(2) 0.4786(2) 0.86759(13) 0.0175(4) Uani 1 1 d . . . . .
C2 C 1.0085(3) 0.7447(3) 0.60655(14) 0.0248(5) Uani 1 1 d . . . . .
C1 C 0.8100(3) 0.9808(3) 0.58241(15) 0.0279(5) Uani 1 1 d . . . . .
C19 C 0.5385(3) 0.7184(3) 0.53021(15) 0.0292(5) Uani 1 1 d . . . . .
H19 H 0.434691 0.757009 0.548086 0.035 Uiso 1 1 calc R U . . .
C17 C 0.3742(3) 0.6157(2) 0.75809(15) 0.0241(5) Uani 1 1 d . . . . .
H17A H 0.374877 0.586972 0.702406 0.036 Uiso 1 1 calc R U . . .
H17B H 0.271193 0.603573 0.785765 0.036 Uiso 1 1 calc R U . . .
H17C H 0.458181 0.547295 0.790563 0.036 Uiso 1 1 calc R U . . .
C18 C 0.6355(3) 0.8000(3) 0.46929(15) 0.0332(6) Uani 1 1 d . . . . .
H18 H 0.607519 0.902650 0.439840 0.040 Uiso 1 1 calc R U . . .
C20 C 0.6258(3) 0.5677(3) 0.55950(16) 0.0312(5) Uani 1 1 d . . . . .
H20 H 0.590109 0.489641 0.600579 0.037 Uiso 1 1 calc R U . . .
C21 C 0.7763(3) 0.5554(3) 0.51604(16) 0.0347(6) Uani 1 1 d . . . . .
H21 H 0.857073 0.467453 0.522892 0.042 Uiso 1 1 calc R U . . .
C8 C 0.9106(3) 0.2371(3) 0.96171(16) 0.0333(6) Uani 1 1 d . . . . .
H8A H 1.019954 0.199525 0.945549 0.050 Uiso 1 1 calc R U . . .
H8B H 0.849144 0.149208 0.971251 0.050 Uiso 1 1 calc R U . . .
H8C H 0.910471 0.282774 1.012803 0.050 Uiso 1 1 calc R U . . .
C15 C 0.2691(3) 1.2161(3) 0.77673(17) 0.0305(5) Uani 1 1 d . . . . .
H15A H 0.225873 1.203437 0.833787 0.046 Uiso 1 1 calc R U . . .
H15B H 0.181950 1.237564 0.737706 0.046 Uiso 1 1 calc R U . . .
H15C H 0.331019 1.303696 0.767902 0.046 Uiso 1 1 calc R U . . .
C14 C 0.6445(3) 1.1802(3) 0.74821(17) 0.0298(5) Uani 1 1 d . . . . .
H14A H 0.738241 1.135246 0.780877 0.045 Uiso 1 1 calc R U . . .
H14B H 0.586621 1.268010 0.772809 0.045 Uiso 1 1 calc R U . . .
H14C H 0.677527 1.217718 0.691037 0.045 Uiso 1 1 calc R U . . .
C22 C 0.7832(3) 0.6992(4) 0.46042(15) 0.0376(6) Uani 1 1 d . . . . .
H22 H 0.869577 0.723774 0.424211 0.045 Uiso 1 1 calc R U . . .
C16 C 0.1240(2) 0.9180(3) 0.78711(17) 0.0298(5) Uani 1 1 d . . . . .
H16A H 0.061986 0.985869 0.742841 0.045 Uiso 1 1 calc R U . . .
H16B H 0.099288 0.958076 0.839707 0.045 Uiso 1 1 calc R U . . .
H16C H 0.097374 0.811355 0.792432 0.045 Uiso 1 1 calc R U . . .
C9 C 0.5470(4) 0.7049(4) 1.03436(17) 0.0451(7) Uani 1 1 d . . . . .
H9A H 0.502401 0.815428 1.032558 0.068 Uiso 1 1 calc R U . . .
H9B H 0.640994 0.681138 1.068828 0.068 Uiso 1 1 calc R U . . .
H9C H 0.467680 0.638620 1.058122 0.068 Uiso 1 1 calc R U . . .


_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 As1 2.5110(3) . ?
Mo1 C3 2.244(2) . ?
Mo1 C2 1.956(2) . ?
Mo1 C1 1.973(2) . ?
Mo1 C19 2.376(2) . ?
Mo1 C18 2.357(2) . ?
Mo1 C20 2.334(2) . ?
Mo1 C21 2.306(2) . ?
Mo1 C22 2.313(2) . ?
As1 C5 1.9415(19) . ?
As1 C10 1.9243(19) . ?
As1 C13 1.9247(18) . ?
O3 C3 1.216(2) . ?
O6 C7 1.196(2) . ?
O5 C6 1.333(2) . ?
O5 C8 1.456(3) . ?
O7 C7 1.330(2) . ?
O7 C9 1.451(3) . ?
O4 C6 1.193(2) . ?
O2 C2 1.151(3) . ?
C5 C4 1.331(3) . ?
C5 C7 1.481(3) . ?
O1 C1 1.153(3) . ?
C4 C3 1.535(3) . ?
C4 C6 1.503(3) . ?
C10 C11 1.344(3) . ?
C10 C14 1.494(3) . ?
C13 C12 1.339(3) . ?
C13 C17 1.493(3) . ?
C12 C11 1.493(3) . ?
C12 C16 1.509(3) . ?
C11 C15 1.501(3) . ?
C19 H19 0.9300 . ?
C19 C18 1.401(3) . ?
C19 C20 1.406(3) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18 0.9300 . ?
C18 C22 1.413(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.405(3) . ?
C21 H21 0.9300 . ?
C21 C22 1.405(4) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C22 H22 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?

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
C3 Mo1 As1 74.63(5) . . ?
C3 Mo1 C19 116.05(8) . . ?
C3 Mo1 C18 143.86(8) . . ?
C3 Mo1 C20 86.46(8) . . ?
C3 Mo1 C21 89.64(9) . . ?
C3 Mo1 C22 122.68(9) . . ?
C2 Mo1 As1 113.81(7) . . ?
C2 Mo1 C3 72.01(8) . . ?
C2 Mo1 C1 75.65(10) . . ?
C2 Mo1 C19 153.41(9) . . ?
C2 Mo1 C18 124.88(9) . . ?
C2 Mo1 C20 129.69(9) . . ?
C2 Mo1 C21 98.19(9) . . ?
C2 Mo1 C22 95.76(9) . . ?
C1 Mo1 As1 79.73(7) . . ?
C1 Mo1 C3 125.17(9) . . ?
C1 Mo1 C19 112.76(9) . . ?
C1 Mo1 C18 90.96(10) . . ?
C1 Mo1 C20 146.87(9) . . ?
C1 Mo1 C21 138.38(10) . . ?
C1 Mo1 C22 103.39(10) . . ?
C19 Mo1 As1 92.72(6) . . ?
C18 Mo1 As1 115.83(6) . . ?
C18 Mo1 C19 34.45(8) . . ?
C20 Mo1 As1 102.67(6) . . ?
C20 Mo1 C19 34.71(8) . . ?
C20 Mo1 C18 57.87(9) . . ?
C21 Mo1 As1 136.83(7) . . ?
C21 Mo1 C19 58.19(8) . . ?
C21 Mo1 C18 58.44(9) . . ?
C21 Mo1 C20 35.24(9) . . ?
C21 Mo1 C22 35.40(10) . . ?
C22 Mo1 As1 149.87(6) . . ?
C22 Mo1 C19 58.11(8) . . ?
C22 Mo1 C18 35.20(9) . . ?
C22 Mo1 C20 58.53(10) . . ?
C5 As1 Mo1 104.48(6) . . ?
C10 As1 Mo1 130.89(6) . . ?
C10 As1 C5 107.81(9) . . ?
C10 As1 C13 89.16(8) . . ?
C13 As1 Mo1 120.78(6) . . ?
C13 As1 C5 99.46(8) . . ?
C6 O5 C8 115.87(17) . . ?
C7 O7 C9 115.63(19) . . ?
C4 C5 As1 112.28(15) . . ?
C4 C5 C7 127.28(18) . . ?
C7 C5 As1 120.21(14) . . ?
C5 C4 C3 120.62(18) . . ?
C5 C4 C6 122.21(19) . . ?
C6 C4 C3 117.14(16) . . ?
C11 C10 As1 107.92(14) . . ?
C11 C10 C14 128.96(19) . . ?
C14 C10 As1 123.10(15) . . ?
O3 C3 Mo1 120.98(15) . . ?
O3 C3 C4 115.90(18) . . ?
C4 C3 Mo1 123.11(13) . . ?
C12 C13 As1 108.82(14) . . ?
C12 C13 C17 130.37(18) . . ?
C17 C13 As1 120.73(14) . . ?
O6 C7 O7 124.8(2) . . ?
O6 C7 C5 124.29(19) . . ?
O7 C7 C5 110.85(17) . . ?
C13 C12 C11 116.20(17) . . ?
C13 C12 C16 124.23(19) . . ?
C11 C12 C16 119.55(18) . . ?
C10 C11 C12 117.32(17) . . ?
C10 C11 C15 123.98(19) . . ?
C12 C11 C15 118.69(18) . . ?
O5 C6 C4 110.74(17) . . ?
O4 C6 O5 125.24(19) . . ?
O4 C6 C4 124.01(18) . . ?
O2 C2 Mo1 177.7(2) . . ?
O1 C1 Mo1 176.4(2) . . ?
Mo1 C19 H19 122.6 . . ?
C18 C19 Mo1 72.03(13) . . ?
C18 C19 H19 126.1 . . ?
C18 C19 C20 107.9(2) . . ?
C20 C19 Mo1 71.03(13) . . ?
C20 C19 H19 126.1 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Mo1 C18 H18 121.5 . . ?
C19 C18 Mo1 73.52(13) . . ?
C19 C18 H18 126.0 . . ?
C19 C18 C22 108.1(2) . . ?
C22 C18 Mo1 70.73(13) . . ?
C22 C18 H18 126.0 . . ?
Mo1 C20 H20 120.3 . . ?
C19 C20 Mo1 74.26(13) . . ?
C19 C20 H20 125.9 . . ?
C21 C20 Mo1 71.29(14) . . ?
C21 C20 C19 108.3(2) . . ?
C21 C20 H20 125.9 . . ?
Mo1 C21 H21 119.8 . . ?
C20 C21 Mo1 73.47(14) . . ?
C20 C21 H21 126.0 . . ?
C22 C21 Mo1 72.59(14) . . ?
C22 C21 C20 107.9(2) . . ?
C22 C21 H21 126.0 . . ?
O5 C8 H8A 109.5 . . ?
O5 C8 H8B 109.5 . . ?
O5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Mo1 C22 H22 119.7 . . ?
C18 C22 Mo1 74.06(14) . . ?
C18 C22 H22 126.1 . . ?
C21 C22 Mo1 72.01(14) . . ?
C21 C22 C18 107.8(2) . . ?
C21 C22 H22 126.1 . . ?
C12 C16 H16A 109.5 . . ?
C12 C16 H16B 109.5 . . ?
C12 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O7 C9 H9A 109.5 . . ?
O7 C9 H9B 109.5 . . ?
O7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 C19 C18 C22 62.70(17) . . . . ?
Mo1 C19 C20 C21 -63.64(16) . . . . ?
Mo1 C18 C22 C21 64.60(17) . . . . ?
Mo1 C20 C21 C22 -64.90(17) . . . . ?
Mo1 C21 C22 C18 -65.95(17) . . . . ?
As1 C5 C4 C3 4.1(2) . . . . ?
As1 C5 C4 C6 -173.76(14) . . . . ?
As1 C5 C7 O6 -81.0(2) . . . . ?
As1 C5 C7 O7 98.06(18) . . . . ?
As1 C10 C11 C12 6.7(2) . . . . ?
As1 C10 C11 C15 -174.58(18) . . . . ?
As1 C13 C12 C11 -3.7(2) . . . . ?
As1 C13 C12 C16 178.19(18) . . . . ?
C5 C4 C3 Mo1 14.9(2) . . . . ?
C5 C4 C3 O3 -164.38(19) . . . . ?
C5 C4 C6 O5 91.5(2) . . . . ?
C5 C4 C6 O4 -88.4(3) . . . . ?
C4 C5 C7 O6 105.0(3) . . . . ?
C4 C5 C7 O7 -75.9(3) . . . . ?
C3 C4 C6 O5 -86.5(2) . . . . ?
C3 C4 C6 O4 93.6(2) . . . . ?
C13 C12 C11 C10 -2.2(3) . . . . ?
C13 C12 C11 C15 179.1(2) . . . . ?
C7 C5 C4 C3 178.52(18) . . . . ?
C7 C5 C4 C6 0.6(3) . . . . ?
C6 C4 C3 Mo1 -167.06(13) . . . . ?
C6 C4 C3 O3 13.6(3) . . . . ?
C19 C18 C22 Mo1 -64.51(17) . . . . ?
C19 C18 C22 C21 0.1(3) . . . . ?
C19 C20 C21 Mo1 65.58(17) . . . . ?
C19 C20 C21 C22 0.7(3) . . . . ?
C17 C13 C12 C11 173.0(2) . . . . ?
C17 C13 C12 C16 -5.2(4) . . . . ?
C18 C19 C20 Mo1 63.01(17) . . . . ?
C18 C19 C20 C21 -0.6(3) . . . . ?
C20 C19 C18 Mo1 -62.37(16) . . . . ?
C20 C19 C18 C22 0.3(3) . . . . ?
C20 C21 C22 Mo1 65.48(17) . . . . ?
C20 C21 C22 C18 -0.5(3) . . . . ?
C8 O5 C6 O4 2.7(3) . . . . ?
C8 O5 C6 C4 -177.22(19) . . . . ?
C14 C10 C11 C12 -174.7(2) . . . . ?
C14 C10 C11 C15 4.0(4) . . . . ?
C16 C12 C11 C10 176.0(2) . . . . ?
C16 C12 C11 C15 -2.7(3) . . . . ?
C9 O7 C7 O6 -1.6(3) . . . . ?
C9 O7 C7 C5 179.3(2) . . . . ?


_ins_header                      
;
TITL RMK_225_E_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 0.71073   8.355720   8.553967  15.982212  80.7685  87.2054  81.5525
ZERR    2.00   0.000265   0.000249   0.000585   0.0027   0.0028   0.0025
LATT  1
SFAC C H O As Mo
UNIT 44.00 46.00 14.00 2.00 2.00
TREF
HKLF 4
END
;
_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 1.474
_oxdiff_exptl_absorpt_empirical_full_min 0.884
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Et2O'
####################################################################### 
# 
# 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_rmk_233_a_scale
_database_code_depnum_ccdc_archive 'CCDC 2145364'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2022-01-29 deposited with the CCDC.	2024-06-27 downloaded from the CCDC.
;
_audit_creation_date             2022-01-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H17 As F6 Mo O3'
_chemical_formula_sum            'C20 H17 As F6 Mo O3'
_chemical_formula_weight         590.20
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H17As1O3Mo1F6
_chemical_oxdiff_usercomment     'Et2O evap at -30 '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   8.62420(10)
_cell_length_b                   17.9549(2)
_cell_length_c                   14.1123(2)
_cell_angle_alpha                90
_cell_angle_beta                 103.3860(10)
_cell_angle_gamma                90
_cell_volume                     2125.87(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8558
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6210
_cell_measurement_theta_min      5.7960
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.451
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.333
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1160
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 -4 -4 0.0774
0 4 8 0.0231
0 -4 -8 0.0701
3 4 5 0.0224
0 -12 1 0.0258
0 12 0 0.0202
1 12 -1 0.0148

_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.052
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-3.9971 -4.3175 -3.7777 0.8805 0.3666 -0.3005
0.0297 3.8883 8.3918 -0.8072 -0.3340 -0.4867
0.0965 -3.8350 -8.4526 0.7966 0.3296 0.5067
3.3977 4.4581 4.9206 -0.9121 -0.3793 0.1555
-0.0064 -11.6070 0.8597 0.6491 -0.7582 -0.0622
-0.0270 11.6569 0.2775 -0.7261 0.6876 -0.0090
0.6493 11.5698 -0.6478 -0.7194 0.6817 0.1332

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13901
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.748
_diffrn_reflns_theta_min         4.053
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     39.00  97.00   1.00    1.00    --   36.95  57.00-120.00   58
  2  ω     55.00  89.00   1.00    1.00    --   36.95-125.00   0.00   34
  3  ω     18.00  67.00   1.00    1.00    --   36.95  38.00-180.00   49
  4  ω     53.00  91.00   1.00    1.00    --   36.95  57.00  90.00   38
  5  ω     -7.00  57.00   1.00    1.00    --   36.95 -77.00 150.00   64
  6  ω     49.00  80.00   1.00    1.00    --   36.95-125.00  90.00   31
  7  ω     32.00 105.00   1.00    1.00    --   36.95  38.00  90.00   73
  8  ω     30.00  77.00   1.00    1.00    --   36.95  38.00-150.00   47
  9  ω    103.00 177.00   1.00    4.00    --  111.00  77.00-150.00   74
 10  ω     73.00 109.00   1.00    4.00    --  111.00-111.00 -30.00   36
 11  ω    145.00 177.00   1.00    4.00    --  111.00  77.00-180.00   32
 12  ω     61.00  88.00   1.00    4.00    --  111.00-111.00-150.00   27
 13  ω    142.00 168.00   1.00    4.00    --  111.00  38.00 120.00   26
 14  ω     95.00 131.00   1.00    4.00    --  111.00  50.00  90.00   36
 15  ω    103.00 177.00   1.00    4.00    --  111.00  77.00 -90.00   74
 16  ω     50.00 109.00   1.00    4.00    --  111.00-111.00  60.00   59
 17  ω     74.00  99.00   1.00    4.00    --  111.00  12.00  30.00   25
 18  ω     74.00 100.00   1.00    4.00    --  111.00 -92.00-120.00   26
 19  ω     81.00 108.00   1.00    4.00    --  111.00-111.00  30.00   27
 20  ω    143.00 171.00   1.00    4.00    --  111.00  12.00  30.00   28
 21  ω     43.00  68.00   1.00    4.00    --  111.00-111.00  30.00   25
 22  ω     61.00 129.00   1.00    4.00    --  111.00 -38.00  90.00   68
 23  ω     63.00 109.00   1.00    4.00    --  111.00-111.00 -90.00   46
 24  ω     84.00 133.00   1.00    4.00    --  111.00 -77.00  90.00   49
 25  ω     84.00 109.00   1.00    4.00    --  111.00-111.00 150.00   25
 26  ω    122.00 175.00   1.00    4.00    --  111.00  50.00 -30.00   53
 27  ω    105.00 146.00   1.00    4.00    --  111.00  64.00-120.00   41
 28  ω    134.00 159.00   1.00    4.00    --  111.00 111.00-120.00   25
 29  ω     96.00 129.00   1.00    4.00    --  111.00 178.00  60.00   33
 30  ω    103.00 128.00   1.00    4.00    --  111.00 178.00 -90.00   25
 31  ω     80.00 109.00   1.00    4.00    --  111.00-111.00   0.00   29
 32  ω     42.00  69.00   1.00    4.00    --  111.00 -92.00-120.00   27
 33  ω     64.00 124.00   1.00    4.00    --  111.00 -64.00 -90.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0905806000
_diffrn_orient_matrix_UB_12      -0.0608838000
_diffrn_orient_matrix_UB_13      -0.0676549000
_diffrn_orient_matrix_UB_21      -0.0931891000
_diffrn_orient_matrix_UB_22      0.0603749000
_diffrn_orient_matrix_UB_23      -0.0674471000
_diffrn_orient_matrix_UB_31      0.1298390000
_diffrn_orient_matrix_UB_32      0.0009274000
_diffrn_orient_matrix_UB_33      -0.0588911000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4044
_reflns_number_total             4288
_reflns_odcompleteness_completeness 98.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.060
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4288
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0420
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0833P)²+0.7784P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1066
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C17(H17), C16(H16), C20(H20)
2.b Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C15(H15a,H15b,H15c), C12(H12a,H12b,H12c), C14(H14a,H14b,
 H14c)
;
_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 0.68566(2) 0.65225(2) 0.49191(2) 0.01116(11) Uani 1 1 d . . . . .
As1 As 0.77149(3) 0.78575(2) 0.52233(2) 0.01042(11) Uani 1 1 d . . . . .
F1 F 0.4401(2) 0.70779(13) 0.75065(15) 0.0291(5) Uani 1 1 d . . . . .
F2 F 0.6519(3) 0.75070(13) 0.84792(13) 0.0297(5) Uani 1 1 d . . . . .
F4 F 0.7450(3) 0.89619(12) 0.77651(15) 0.0316(5) Uani 1 1 d . . . . .
F3 F 0.4786(3) 0.82530(13) 0.76158(16) 0.0323(5) Uani 1 1 d . . . . .
O3 O 0.6786(3) 0.62861(13) 0.70369(17) 0.0254(5) Uani 1 1 d . . . . .
O2 O 0.3294(3) 0.63933(15) 0.50066(19) 0.0257(5) Uani 1 1 d . . . . .
F5 F 0.8490(4) 0.92458(13) 0.6581(2) 0.0506(8) Uani 1 1 d . . . . .
F6 F 0.5949(4) 0.93291(14) 0.6410(2) 0.0527(8) Uani 1 1 d . . . . .
O1 O 0.5152(3) 0.72487(16) 0.29287(17) 0.0323(6) Uani 1 1 d . . . . .
C6 C 0.5538(4) 0.75994(19) 0.7604(2) 0.0194(6) Uani 1 1 d . . . . .
C5 C 0.7049(3) 0.81306(16) 0.6421(2) 0.0144(5) Uani 1 1 d . . . . .
C3 C 0.6656(3) 0.67680(16) 0.6425(2) 0.0146(5) Uani 1 1 d . . . . .
C4 C 0.6395(3) 0.75583(16) 0.6781(2) 0.0139(5) Uani 1 1 d . . . . .
C9 C 0.9732(3) 0.87692(16) 0.4626(2) 0.0159(5) Uani 1 1 d . . . . .
C2 C 0.4599(4) 0.64463(15) 0.4964(2) 0.0156(6) Uani 1 1 d . . . . .
C1 C 0.5781(4) 0.70015(18) 0.3674(2) 0.0206(6) Uani 1 1 d . . . . .
C11 C 0.6873(4) 0.86644(17) 0.4346(2) 0.0169(5) Uani 1 1 d . . . . .
C8 C 0.9834(3) 0.82152(17) 0.5274(2) 0.0163(6) Uani 1 1 d . . . . .
C10 C 0.8107(4) 0.90120(16) 0.4108(2) 0.0176(6) Uani 1 1 d . . . . .
C7 C 0.7231(5) 0.89171(18) 0.6798(2) 0.0262(7) Uani 1 1 d . . . . .
C13 C 1.1163(4) 0.9155(2) 0.4411(3) 0.0277(7) Uani 1 1 d . . . . .
H13A H 1.211705 0.895588 0.482246 0.042 Uiso 1 1 calc GR . . . .
H13B H 1.110107 0.967943 0.453125 0.042 Uiso 1 1 calc GR . . . .
H13C H 1.118277 0.907666 0.374061 0.042 Uiso 1 1 calc GR . . . .
C15 C 0.5124(4) 0.8808(2) 0.4002(3) 0.0283(7) Uani 1 1 d . . . . .
H15A H 0.453936 0.840116 0.419161 0.042 Uiso 1 1 calc GR . . . .
H15B H 0.485535 0.885378 0.330514 0.042 Uiso 1 1 calc GR . . . .
H15C H 0.485413 0.926084 0.428771 0.042 Uiso 1 1 calc GR . . . .
C18 C 0.7141(4) 0.53120(17) 0.4406(3) 0.0253(7) Uani 1 1 d . . . . .
H18 H 0.625885 0.505325 0.405556 0.030 Uiso 1 1 calc R . . . .
C19 C 0.7668(5) 0.53356(18) 0.5431(3) 0.0279(7) Uani 1 1 d . . . . .
H19 H 0.719485 0.509522 0.587539 0.033 Uiso 1 1 calc R . . . .
C17 C 0.8196(4) 0.57531(17) 0.4007(3) 0.0254(7) Uani 1 1 d . . . . .
H17 H 0.812026 0.583352 0.334639 0.031 Uiso 1 1 calc R . . . .
C12 C 1.1306(4) 0.7861(2) 0.5885(3) 0.0250(7) Uani 1 1 d . . . . .
H12A H 1.178033 0.819013 0.640806 0.037 Uiso 1 1 calc GR . . . .
H12B H 1.205229 0.776507 0.548977 0.037 Uiso 1 1 calc GR . . . .
H12C H 1.102699 0.740015 0.614901 0.037 Uiso 1 1 calc GR . . . .
C16 C 0.9376(4) 0.6049(2) 0.4772(3) 0.0294(7) Uani 1 1 d . . . . .
H16 H 1.021403 0.635551 0.470751 0.035 Uiso 1 1 calc R . . . .
C14 C 0.7903(5) 0.9619(2) 0.3352(3) 0.0324(8) Uani 1 1 d . . . . .
H14A H 0.842203 1.006375 0.364251 0.049 Uiso 1 1 calc GR . . . .
H14B H 0.678822 0.971606 0.310335 0.049 Uiso 1 1 calc GR . . . .
H14C H 0.836854 0.946343 0.282894 0.049 Uiso 1 1 calc GR . . . .
C20 C 0.9057(4) 0.5795(2) 0.5662(3) 0.0309(8) Uani 1 1 d . . . . .
H20 H 0.964844 0.590796 0.628425 0.037 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 As1 2.5161(4) . ?
Mo1 C3 2.216(3) . ?
Mo1 C2 1.967(3) . ?
Mo1 C1 1.983(3) . ?
Mo1 C18 2.322(3) . ?
Mo1 C19 2.306(3) . ?
Mo1 C17 2.364(3) . ?
Mo1 C16 2.386(3) . ?
Mo1 C20 2.342(3) . ?
As1 C5 1.969(3) . ?
As1 C11 1.934(3) . ?
As1 C8 1.923(3) . ?
F1 C6 1.340(4) . ?
F2 C6 1.335(4) . ?
F4 C7 1.336(4) . ?
F3 C6 1.343(4) . ?
O3 C3 1.209(4) . ?
O2 C2 1.145(4) . ?
F5 C7 1.332(4) . ?
F6 C7 1.337(5) . ?
O1 C1 1.155(4) . ?
C6 C4 1.516(4) . ?
C5 C4 1.329(4) . ?
C5 C7 1.504(4) . ?
C3 C4 1.539(4) . ?
C9 C8 1.340(4) . ?
C9 C10 1.488(4) . ?
C9 C13 1.507(4) . ?
C11 C10 1.341(4) . ?
C11 C15 1.497(4) . ?
C8 C12 1.501(4) . ?
C10 C14 1.506(4) . ?
C18 C19 1.413(5) . ?
C18 C17 1.418(4) . ?
C19 C20 1.429(5) . ?
C17 C16 1.405(5) . ?
C16 C20 1.421(6) . ?

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
C3 Mo1 As1 74.46(8) . . ?
C3 Mo1 C18 121.51(12) . . ?
C3 Mo1 C19 88.22(12) . . ?
C3 Mo1 C17 142.66(12) . . ?
C3 Mo1 C16 115.42(13) . . ?
C3 Mo1 C20 85.23(12) . . ?
C2 Mo1 As1 108.36(8) . . ?
C2 Mo1 C3 71.67(11) . . ?
C2 Mo1 C1 78.19(12) . . ?
C2 Mo1 C18 96.99(12) . . ?
C2 Mo1 C19 99.00(13) . . ?
C2 Mo1 C17 126.08(12) . . ?
C2 Mo1 C16 154.91(12) . . ?
C2 Mo1 C20 130.71(13) . . ?
C1 Mo1 As1 78.27(9) . . ?
C1 Mo1 C3 129.72(12) . . ?
C1 Mo1 C18 101.02(13) . . ?
C1 Mo1 C19 136.39(14) . . ?
C1 Mo1 C17 87.60(13) . . ?
C1 Mo1 C16 109.02(13) . . ?
C1 Mo1 C20 143.39(13) . . ?
C18 Mo1 As1 153.75(8) . . ?
C18 Mo1 C17 35.21(11) . . ?
C18 Mo1 C16 58.34(12) . . ?
C18 Mo1 C20 58.97(13) . . ?
C19 Mo1 As1 140.44(10) . . ?
C19 Mo1 C18 35.55(13) . . ?
C19 Mo1 C17 58.64(12) . . ?
C19 Mo1 C16 58.78(13) . . ?
C19 Mo1 C20 35.80(14) . . ?
C17 Mo1 As1 119.20(8) . . ?
C17 Mo1 C16 34.40(13) . . ?
C16 Mo1 As1 96.69(9) . . ?
C20 Mo1 As1 106.20(10) . . ?
C20 Mo1 C17 58.03(13) . . ?
C20 Mo1 C16 34.97(14) . . ?
C5 As1 Mo1 104.53(9) . . ?
C11 As1 Mo1 123.54(9) . . ?
C11 As1 C5 102.83(12) . . ?
C8 As1 Mo1 124.34(9) . . ?
C8 As1 C5 110.37(12) . . ?
C8 As1 C11 89.22(13) . . ?
F1 C6 F3 105.5(3) . . ?
F1 C6 C4 111.2(3) . . ?
F2 C6 F1 107.5(3) . . ?
F2 C6 F3 107.6(3) . . ?
F2 C6 C4 112.7(3) . . ?
F3 C6 C4 112.0(3) . . ?
C4 C5 As1 111.7(2) . . ?
C4 C5 C7 127.6(3) . . ?
C7 C5 As1 120.7(2) . . ?
O3 C3 Mo1 121.8(2) . . ?
O3 C3 C4 115.0(3) . . ?
C4 C3 Mo1 123.12(19) . . ?
C6 C4 C3 115.4(2) . . ?
C5 C4 C6 125.5(3) . . ?
C5 C4 C3 118.7(2) . . ?
C8 C9 C10 117.3(3) . . ?
C8 C9 C13 123.5(3) . . ?
C10 C9 C13 119.2(3) . . ?
O2 C2 Mo1 178.6(3) . . ?
O1 C1 Mo1 176.8(3) . . ?
C10 C11 As1 107.9(2) . . ?
C10 C11 C15 129.5(3) . . ?
C15 C11 As1 122.5(2) . . ?
C9 C8 As1 108.1(2) . . ?
C9 C8 C12 128.3(3) . . ?
C12 C8 As1 123.4(2) . . ?
C9 C10 C14 120.1(3) . . ?
C11 C10 C9 116.8(3) . . ?
C11 C10 C14 123.0(3) . . ?
F4 C7 F6 107.0(3) . . ?
F4 C7 C5 113.3(3) . . ?
F5 C7 F4 106.2(3) . . ?
F5 C7 F6 107.6(3) . . ?
F5 C7 C5 111.0(3) . . ?
F6 C7 C5 111.5(3) . . ?
C19 C18 Mo1 71.62(18) . . ?
C19 C18 C17 107.8(3) . . ?
C17 C18 Mo1 74.04(17) . . ?
C18 C19 Mo1 72.83(18) . . ?
C18 C19 C20 107.8(3) . . ?
C20 C19 Mo1 73.48(18) . . ?
C18 C17 Mo1 70.75(17) . . ?
C16 C17 Mo1 73.66(18) . . ?
C16 C17 C18 108.8(3) . . ?
C17 C16 Mo1 71.94(18) . . ?
C17 C16 C20 107.7(3) . . ?
C20 C16 Mo1 70.81(17) . . ?
C19 C20 Mo1 70.72(18) . . ?
C16 C20 Mo1 74.22(19) . . ?
C16 C20 C19 107.8(3) . . ?


_ins_header                      
;
TITL RMK_233_A_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184   8.624161  17.954878  14.112303  90.0000 103.3861  90.0000
ZERR    4.00   0.000111   0.000237   0.000179   0.0000   0.0013   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H O F As Mo
UNIT 80.00 68.00 12.00 24.00 4.00 4.00
TREF
HKLF 4
END
;
_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 1.613
_oxdiff_exptl_absorpt_empirical_full_min 0.709
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Et2O'
####################################################################### 
# 
# 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_rmk_219_c_scale
_database_code_depnum_ccdc_archive 'CCDC 2145381'
loop_
_audit_author_name
_audit_author_address
'Ryan Kirk'
;Australian National University 
Australia
;
_audit_update_record             
;
2022-01-29 deposited with the CCDC.	2024-06-27 downloaded from the CCDC.
;
_audit_creation_date             2022-01-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I, C10 H18 As'
_chemical_formula_sum            'C10 H18 As I'
_chemical_formula_weight         340.06
_chemical_melting_point          ?
_chemical_oxdiff_formula         C10H18As1I1
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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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                   7.9883(4)
_cell_length_b                   7.6338(3)
_cell_length_c                   21.1208(8)
_cell_angle_alpha                90
_cell_angle_beta                 91.549(4)
_cell_angle_gamma                90
_cell_volume                     1287.50(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8577
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      31.9870
_cell_measurement_theta_min      3.6540
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.995
_exptl_absorpt_correction_T_max  0.50085
_exptl_absorpt_correction_T_min  0.48902
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
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    1.754
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             656
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
11 1 -7 0.0402
-11 0 8 0.0334
0 -11 -2 0.1436
-4 10 4 0.1264
-2 0 -29 0.0282
2 0 29 0.0282

_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.056
_exptl_crystal_size_rad          0.065
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
10.9401 0.8534 -7.4392 0.6960 0.5948 0.4023
-10.9611 0.0389 7.6089 -0.7190 -0.6144 -0.3248
-0.4573 -10.7386 -1.5491 0.2305 0.1964 -0.9531
-3.6218 10.0855 4.2647 -0.4818 -0.4112 0.7738
-1.6797 -0.2546 -29.3071 -0.5657 0.8229 -0.0535
1.6797 0.2546 29.3071 0.5657 -0.8229 0.0535

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            24274
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.410
_diffrn_reflns_theta_min         3.240
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -94.00 -22.00   1.00   60.00    --  -17.53 155.00   0.72   72
  2  ω    -93.00 -33.00   1.00   60.00    --  -17.53 153.00 -99.35   60
  3  ω    -22.00  97.00   1.00   60.00    --   17.84  19.00-120.00  119
  4  ω     -6.00  92.00   1.00   60.00    --   17.84  37.00 -30.00   98
  5  ω     -5.00  42.00   1.00   60.00    --   17.84  77.00 150.00   47
  6  ω    -36.00  50.00   1.00   60.00    --   17.84 -77.00 -90.00   86
  7  ω    -40.00  49.00   1.00   60.00    --   17.84 -77.00-180.00   89
  8  ω     -9.00  41.00   1.00   60.00    --   17.84  57.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0760374000
_diffrn_orient_matrix_UB_12      -0.0268874000
_diffrn_orient_matrix_UB_13      0.0151765000
_diffrn_orient_matrix_UB_21      0.0351987000
_diffrn_orient_matrix_UB_22      -0.0154629000
_diffrn_orient_matrix_UB_23      -0.0299617000
_diffrn_orient_matrix_UB_31      0.0295121000
_diffrn_orient_matrix_UB_32      0.0875851000
_diffrn_orient_matrix_UB_33      -0.0006259000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\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                3488
_reflns_number_total             4258
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.51
_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 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         4258
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0322
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0178P)²+1.0580P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0583
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C2(H2a,H2b,H2c), C8(H8a,H8b,H8c), C1(H1a,H1b,H1c), C9(H9a,
 H9b,H9c), C10(H10a,H10b,H10c)
;
_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
I1 I 0.30310(2) 0.48494(2) 0.84891(2) 0.03138(6) Uani 1 1 d . . . . .
As1 As 0.32858(3) 0.42698(3) 0.64042(2) 0.02042(6) Uani 1 1 d . . . . .
C3 C 0.3314(3) 0.3858(3) 0.55141(12) 0.0228(5) Uani 1 1 d . . . . .
C5 C 0.1843(3) 0.6612(3) 0.56622(13) 0.0229(5) Uani 1 1 d . . . . .
C7 C 0.3988(3) 0.2233(3) 0.52222(13) 0.0287(6) Uani 1 1 d . . . . .
H7A H 0.500333 0.189350 0.544303 0.043 Uiso 1 1 calc R U . . .
H7B H 0.421747 0.245113 0.478537 0.043 Uiso 1 1 calc R U . . .
H7C H 0.317825 0.130959 0.525046 0.043 Uiso 1 1 calc R U . . .
C6 C 0.2059(3) 0.6388(3) 0.62871(13) 0.0241(5) Uani 1 1 d . . . . .
C2 C 0.5364(3) 0.4684(3) 0.68462(13) 0.0263(5) Uani 1 1 d . . . . .
H2A H 0.608353 0.368801 0.679899 0.039 Uiso 1 1 calc R U . . .
H2B H 0.516342 0.486883 0.728733 0.039 Uiso 1 1 calc R U . . .
H2C H 0.588978 0.570334 0.667465 0.039 Uiso 1 1 calc R U . . .
C4 C 0.2487(3) 0.5201(3) 0.52384(12) 0.0221(5) Uani 1 1 d . . . . .
C8 C 0.2143(4) 0.5326(4) 0.45393(13) 0.0300(6) Uani 1 1 d . . . . .
H8A H 0.266817 0.635868 0.437741 0.045 Uiso 1 1 calc R U . . .
H8B H 0.095667 0.538994 0.445793 0.045 Uiso 1 1 calc R U . . .
H8C H 0.258490 0.431026 0.433432 0.045 Uiso 1 1 calc R U . . .
C1 C 0.2094(4) 0.2451(4) 0.68197(14) 0.0344(7) Uani 1 1 d . . . . .
H1A H 0.102537 0.228211 0.660968 0.052 Uiso 1 1 calc R U . . .
H1B H 0.193125 0.277389 0.725299 0.052 Uiso 1 1 calc R U . . .
H1C H 0.272639 0.138311 0.680521 0.052 Uiso 1 1 calc R U . . .
C9 C 0.0983(4) 0.8176(3) 0.53668(14) 0.0328(6) Uani 1 1 d . . . . .
H9A H 0.000744 0.779733 0.512904 0.049 Uiso 1 1 calc R U . . .
H9B H 0.173595 0.875803 0.508954 0.049 Uiso 1 1 calc R U . . .
H9C H 0.065560 0.897025 0.569348 0.049 Uiso 1 1 calc R U . . .
C10 C 0.1609(4) 0.7533(4) 0.68340(14) 0.0373(7) Uani 1 1 d . . . . .
H10A H 0.120149 0.681990 0.717097 0.056 Uiso 1 1 calc R U . . .
H10B H 0.075416 0.834705 0.669986 0.056 Uiso 1 1 calc R U . . .
H10C H 0.258226 0.816622 0.698111 0.056 Uiso 1 1 calc R U . . .


_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
As1 C3 1.907(3) . ?
As1 C6 1.903(2) . ?
As1 C2 1.909(2) . ?
As1 C1 1.910(3) . ?
C3 C7 1.492(4) . ?
C3 C4 1.344(3) . ?
C5 C6 1.337(4) . ?
C5 C4 1.500(4) . ?
C5 C9 1.504(3) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C6 C10 1.500(4) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C4 C8 1.498(4) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?

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
C3 As1 C2 118.43(11) . . ?
C3 As1 C1 110.64(12) . . ?
C6 As1 C3 91.82(11) . . ?
C6 As1 C2 111.14(11) . . ?
C6 As1 C1 114.58(13) . . ?
C2 As1 C1 109.47(12) . . ?
C7 C3 As1 123.95(19) . . ?
C4 C3 As1 106.42(19) . . ?
C4 C3 C7 129.3(2) . . ?
C6 C5 C4 117.4(2) . . ?
C6 C5 C9 123.8(3) . . ?
C4 C5 C9 118.8(2) . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C6 As1 106.82(19) . . ?
C5 C6 C10 131.1(2) . . ?
C10 C6 As1 121.90(19) . . ?
As1 C2 H2A 109.5 . . ?
As1 C2 H2B 109.5 . . ?
As1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 C4 C5 117.5(2) . . ?
C3 C4 C8 123.4(2) . . ?
C8 C4 C5 119.1(2) . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
As1 C1 H1A 109.5 . . ?
As1 C1 H1B 109.5 . . ?
As1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 H10A 109.5 . . ?
C6 C10 H10B 109.5 . . ?
C6 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
As1 C3 C4 C5 1.8(3) . . . . ?
As1 C3 C4 C8 -176.5(2) . . . . ?
C7 C3 C4 C5 175.6(2) . . . . ?
C7 C3 C4 C8 -2.7(4) . . . . ?
C6 C5 C4 C3 -3.5(3) . . . . ?
C6 C5 C4 C8 174.9(2) . . . . ?
C4 C5 C6 As1 3.0(3) . . . . ?
C4 C5 C6 C10 178.6(3) . . . . ?
C9 C5 C6 As1 -177.7(2) . . . . ?
C9 C5 C6 C10 -2.1(5) . . . . ?
C9 C5 C4 C3 177.2(2) . . . . ?
C9 C5 C4 C8 -4.4(3) . . . . ?


_ins_header                      
;
TITL RMK_219_C_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073   7.988313   7.633773  21.120777  90.0000  91.5493  90.0000
ZERR    6.00   0.000384   0.000288   0.000791   0.0000   0.0042   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H As I
UNIT 60.00 108.00 6.00 6.00
TREF
HKLF 4
END
;
_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 1.205
_oxdiff_exptl_absorpt_empirical_full_min 0.890
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: C6D6'
_chemical_properties_physical    Moisture-sensitive
