#------------------------------------------------------------------------------
#$Date: 2024-08-05 21:49:01 +0300 (Mon, 05 Aug 2024) $
#$Revision: 293823 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/65/7716525.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7716525
loop_
_publ_author_name
'Kirk, Ryan M.'
'Hill, Anthony F.'
_publ_section_title
;
 Electrophilic As-functionalisation of σ-arsolido complexes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11959
_journal_page_last               11969
_journal_paper_doi               10.1039/d4dt01371a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C16 H20 As I Mo O2'
_chemical_formula_sum            'C16 H20 As I Mo O2'
_chemical_formula_weight         542.08
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-01-29 deposited with the CCDC.	2024-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                104.867(3)
_cell_angle_beta                 104.316(3)
_cell_angle_gamma                91.742(2)
_cell_formula_units_Z            4
_cell_length_a                   8.8572(3)
_cell_length_b                   13.9206(4)
_cell_length_c                   16.0715(5)
_cell_measurement_reflns_used    7113
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.1350
_cell_measurement_theta_min      5.1620
_cell_volume                     1846.43(11)
_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)'
_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_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_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_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_description       prism
_exptl_crystal_F_000             1040
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.142
_exptl_crystal_size_rad          0.101
_refine_diff_density_max         1.133
_refine_diff_density_min         -1.637
_refine_diff_density_rms         0.164
_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_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0355
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6786
_reflns_number_total             7149
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01371a2.cif
_cod_data_source_block           rmk_219_c_red_a_scale
_cod_depositor_comments
'Adding full bibliography for 7716522--7716529.cif.'
_cod_database_code               7716525
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Mo1As1O3I1C16H20
_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.
;
_reflns_odcompleteness_completeness 95.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.08
_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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 . . .
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'
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
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_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_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) . . . . ?
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
