# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

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#                                CCDC 
# 
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#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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data_3-1697

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
3-1697 [Mo(PNPMe-iPr)(CO)I2], 
Diiodo-carbonyl-[N,N'-bis(diisopropylphosphino)-N,N'-dimethyl-2,6-
diaminopyridine-\kP,N¹,P']-molybdenum(iv)
;
_chemical_name_common            '3-1697 [Mo(PNPMe-iPr)(CO)I2]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H37 I2 Mo N3 O P2'
_chemical_formula_sum            'C20 H37 I2 Mo N3 O P2'
_chemical_formula_weight         747.21

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '

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

_cell_length_a                   20.8211(7)
_cell_length_b                   15.7605(5)
_cell_length_c                   17.6677(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.312(2)
_cell_angle_gamma                90.00
_cell_volume                     5283.5(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9993
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      29.97

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2912
_exptl_absorpt_coefficient_mu    2.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_process_details   'program SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            86452
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         30.00
_reflns_number_total             15409
_reflns_number_gt                12721
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0195P)²+4.3506P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         15409
_refine_ls_number_parameters     564
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0265
_refine_ls_wR_factor_ref         0.0553
_refine_ls_wR_factor_gt          0.0510
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.098418(11) 0.777173(13) 0.179454(13) 0.00888(4) Uani 1 1 d . . .
Mo2 Mo 0.412247(11) 0.229201(14) 0.815885(13) 0.01069(4) Uani 1 1 d . . .
I1 I 0.091566(9) 0.942942(11) 0.226962(11) 0.01570(4) Uani 1 1 d . . .
I2 I 0.211076(9) 0.832537(11) 0.139503(10) 0.01422(4) Uani 1 1 d . . .
I3 I 0.425655(9) 0.073643(11) 0.892701(11) 0.01745(4) Uani 1 1 d . . .
I4 I 0.345656(9) 0.138512(12) 0.663498(11) 0.01853(4) Uani 1 1 d . . .
P1 P -0.00674(3) 0.74497(4) 0.06057(4) 0.01031(12) Uani 1 1 d . . .
P2 P 0.16214(3) 0.68262(4) 0.28970(4) 0.01201(13) Uani 1 1 d . . .
P3 P 0.52208(3) 0.27417(4) 0.81818(4) 0.01235(13) Uani 1 1 d . A .
P4 P 0.32418(4) 0.31873(4) 0.82688(4) 0.01353(13) Uani 1 1 d . A .
N1 N 0.12128(11) 0.65566(13) 0.12552(13) 0.0115(4) Uani 1 1 d . . .
N2 N 0.01680(11) 0.67050(13) 0.00672(13) 0.0124(4) Uani 1 1 d . . .
N3 N 0.21450(11) 0.62955(14) 0.25229(14) 0.0143(4) Uani 1 1 d . . .
N4 N 0.38972(11) 0.33364(13) 0.71943(13) 0.0123(4) Uani 1 1 d . . .
N5 N 0.50029(12) 0.31142(17) 0.72015(14) 0.0213(5) Uani 1 1 d . . .
N6 N 0.28484(12) 0.36394(15) 0.73092(15) 0.0190(5) Uani 1 1 d . . .
O1 O -0.00469(10) 0.76149(13) 0.26351(12) 0.0195(4) Uani 1 1 d . . .
O2 O 0.48951(11) 0.28700(14) 0.99838(11) 0.0248(5) Uani 1 1 d . . .
C1 C 0.08179(13) 0.63219(15) 0.04561(16) 0.0121(5) Uani 1 1 d . . .
C2 C 0.10556(15) 0.57196(17) 0.00489(17) 0.0173(5) Uani 1 1 d . . .
H2 H 0.0785 0.5584 -0.0518 0.021 Uiso 1 1 calc R . .
C3 C 0.16912(15) 0.53286(17) 0.04904(19) 0.0197(6) Uani 1 1 d . . .
H3 H 0.1872 0.4938 0.0217 0.024 Uiso 1 1 calc R . .
C4 C 0.20698(14) 0.54942(17) 0.13202(18) 0.0176(5) Uani 1 1 d . . .
H4 H 0.2494 0.5197 0.1633 0.021 Uiso 1 1 calc R . .
C5 C 0.18145(13) 0.61088(16) 0.16888(16) 0.0130(5) Uani 1 1 d . . .
C6 C -0.03870(14) 0.83311(16) -0.01461(16) 0.0148(5) Uani 1 1 d . . .
H6 H -0.0761 0.8093 -0.0665 0.018 Uiso 1 1 calc R . .
C7 C -0.07325(15) 0.90290(17) 0.01622(18) 0.0206(6) Uani 1 1 d . . .
H7A H -0.0388 0.9256 0.0690 0.031 Uiso 1 1 calc R . .
H7B H -0.1135 0.8792 0.0244 0.031 Uiso 1 1 calc R . .
H7C H -0.0896 0.9486 -0.0250 0.031 Uiso 1 1 calc R . .
C8 C 0.01891(16) 0.86813(19) -0.03789(19) 0.0229(6) Uani 1 1 d . . .
H8A H -0.0013 0.9104 -0.0821 0.034 Uiso 1 1 calc R . .
H8B H 0.0395 0.8218 -0.0574 0.034 Uiso 1 1 calc R . .
H8C H 0.0556 0.8948 0.0109 0.034 Uiso 1 1 calc R . .
C9 C -0.08761(13) 0.70719(17) 0.06870(16) 0.0146(5) Uani 1 1 d . . .
H9 H -0.0980 0.7490 0.1047 0.017 Uiso 1 1 calc R . .
C10 C -0.07393(15) 0.62228(18) 0.11466(17) 0.0200(6) Uani 1 1 d . . .
H10A H -0.1173 0.6027 0.1181 0.030 Uiso 1 1 calc R . .
H10B H -0.0370 0.6295 0.1708 0.030 Uiso 1 1 calc R . .
H10C H -0.0587 0.5803 0.0845 0.030 Uiso 1 1 calc R . .
C11 C -0.15447(14) 0.70150(19) -0.01228(17) 0.0213(6) Uani 1 1 d . . .
H11A H -0.1487 0.6568 -0.0475 0.032 Uiso 1 1 calc R . .
H11B H -0.1625 0.7559 -0.0416 0.032 Uiso 1 1 calc R . .
H11C H -0.1949 0.6882 0.0005 0.032 Uiso 1 1 calc R . .
C12 C 0.22261(14) 0.73611(18) 0.38479(16) 0.0167(5) Uani 1 1 d . . .
H12 H 0.2500 0.6912 0.4251 0.020 Uiso 1 1 calc R . .
C13 C 0.17889(16) 0.78385(19) 0.42295(17) 0.0218(6) Uani 1 1 d . . .
H13A H 0.2101 0.8053 0.4779 0.033 Uiso 1 1 calc R . .
H13B H 0.1441 0.7452 0.4283 0.033 Uiso 1 1 calc R . .
H13C H 0.1545 0.8315 0.3870 0.033 Uiso 1 1 calc R . .
C14 C 0.27547(15) 0.7949(2) 0.37146(17) 0.0224(6) Uani 1 1 d . . .
H14A H 0.2504 0.8428 0.3365 0.034 Uiso 1 1 calc R . .
H14B H 0.3005 0.7634 0.3441 0.034 Uiso 1 1 calc R . .
H14C H 0.3094 0.8160 0.4253 0.034 Uiso 1 1 calc R . .
C15 C 0.11946(14) 0.59786(17) 0.32534(17) 0.0172(5) Uani 1 1 d . . .
H15 H 0.0772 0.6233 0.3298 0.021 Uiso 1 1 calc R . .
C16 C 0.09330(15) 0.52738(18) 0.26006(18) 0.0203(6) Uani 1 1 d . . .
H16A H 0.1337 0.4955 0.2600 0.030 Uiso 1 1 calc R . .
H16B H 0.0671 0.5525 0.2051 0.030 Uiso 1 1 calc R . .
H16C H 0.0623 0.4890 0.2733 0.030 Uiso 1 1 calc R . .
C17 C 0.16555(17) 0.5593(2) 0.41025(18) 0.0258(7) Uani 1 1 d . . .
H17A H 0.1395 0.5139 0.4232 0.039 Uiso 1 1 calc R . .
H17B H 0.1780 0.6034 0.4530 0.039 Uiso 1 1 calc R . .
H17C H 0.2086 0.5359 0.4087 0.039 Uiso 1 1 calc R . .
C18 C -0.02827(15) 0.64365(18) -0.07864(16) 0.0191(6) Uani 1 1 d . . .
H18A H -0.0031 0.6524 -0.1143 0.029 Uiso 1 1 calc R . .
H18B H -0.0717 0.6773 -0.0997 0.029 Uiso 1 1 calc R . .
H18C H -0.0400 0.5834 -0.0787 0.029 Uiso 1 1 calc R . .
C19 C 0.27702(14) 0.58019(19) 0.30408(18) 0.0215(6) Uani 1 1 d . . .
H19A H 0.2638 0.5206 0.3048 0.032 Uiso 1 1 calc R . .
H19B H 0.2965 0.6027 0.3608 0.032 Uiso 1 1 calc R . .
H19C H 0.3125 0.5843 0.2812 0.032 Uiso 1 1 calc R . .
C20 C 0.03365(13) 0.76536(16) 0.23048(15) 0.0128(5) Uani 1 1 d . . .
C21 C 0.43413(14) 0.34641(17) 0.68129(16) 0.0155(5) Uani 1 1 d . . .
C22 C 0.41410(15) 0.39210(19) 0.60805(16) 0.0198(6) Uani 1 1 d . . .
H22 H 0.4452 0.3982 0.5814 0.024 Uiso 1 1 calc R . .
C23 C 0.34811(15) 0.42835(18) 0.57478(16) 0.0185(6) Uani 1 1 d . . .
H23 H 0.3330 0.4586 0.5238 0.022 Uiso 1 1 calc R . .
C24 C 0.30367(15) 0.42128(17) 0.61455(17) 0.0186(6) Uani 1 1 d . . .
H24 H 0.2589 0.4482 0.5930 0.022 Uiso 1 1 calc R . .
C25 C 0.32632(14) 0.37365(16) 0.68706(16) 0.0143(5) Uani 1 1 d . . .
C26 C 0.58494(14) 0.18778(17) 0.83080(17) 0.0177(5) Uani 1 1 d . . .
H26 H 0.6249 0.2126 0.8208 0.021 Uiso 1 1 calc R . .
C27 C 0.61568(15) 0.15440(18) 0.92027(18) 0.0228(6) Uani 1 1 d . . .
H27A H 0.5785 0.1260 0.9313 0.034 Uiso 1 1 calc R . .
H27B H 0.6346 0.2019 0.9589 0.034 Uiso 1 1 calc R . .
H27C H 0.6536 0.1139 0.9277 0.034 Uiso 1 1 calc R . .
C28 C 0.55432(16) 0.1157(2) 0.76816(19) 0.0250(6) Uani 1 1 d . . .
H28A H 0.5921 0.0764 0.7723 0.037 Uiso 1 1 calc R . .
H28B H 0.5327 0.1392 0.7119 0.037 Uiso 1 1 calc R . .
H28C H 0.5185 0.0853 0.7802 0.037 Uiso 1 1 calc R . .
C29 C 0.57688(14) 0.35748(17) 0.88849(18) 0.0185(6) Uani 1 1 d . . .
H29 H 0.5861 0.3394 0.9463 0.022 Uiso 1 1 d R A .
C30A C 0.5382(2) 0.4381(3) 0.8894(4) 0.0213(12) Uani 0.630(7) 1 d P A 1
H30A H 0.5714 0.4792 0.9270 0.032 Uiso 0.630(7) 1 calc PR A 1
H30B H 0.5013 0.4256 0.9087 0.032 Uiso 0.630(7) 1 calc PR A 1
H30C H 0.5168 0.4619 0.8333 0.032 Uiso 0.630(7) 1 calc PR A 1
C30B C 0.5372(4) 0.4437(4) 0.8409(5) 0.0148(17) Uani 0.370(7) 1 d P A 2
H30D H 0.5524 0.4917 0.8795 0.022 Uiso 0.370(7) 1 calc PR A 2
H30E H 0.4861 0.4365 0.8207 0.022 Uiso 0.370(7) 1 calc PR A 2
H30F H 0.5493 0.4548 0.7937 0.022 Uiso 0.370(7) 1 calc PR A 2
C31 C 0.64871(15) 0.3718(2) 0.88681(19) 0.0241(6) Uani 1 1 d . A .
H31A H 0.6423 0.3955 0.8329 0.036 Uiso 1 1 calc R . .
H31B H 0.6739 0.3177 0.8954 0.036 Uiso 1 1 calc R . .
H31C H 0.6761 0.4115 0.9310 0.036 Uiso 1 1 calc R . .
C32 C 0.25206(14) 0.25969(18) 0.83836(17) 0.0171(5) Uani 1 1 d . . .
H32 H 0.2158 0.3021 0.8369 0.021 Uiso 1 1 calc R . .
C33 C 0.27916(18) 0.2155(2) 0.92283(19) 0.0283(7) Uani 1 1 d . . .
H33A H 0.2395 0.1898 0.9307 0.042 Uiso 1 1 calc R . .
H33B H 0.3024 0.2572 0.9669 0.042 Uiso 1 1 calc R . .
H33C H 0.3130 0.1713 0.9251 0.042 Uiso 1 1 calc R . .
C34 C 0.21580(16) 0.1967(2) 0.7671(2) 0.0266(7) Uani 1 1 d . . .
H34A H 0.2501 0.1543 0.7667 0.040 Uiso 1 1 calc R . .
H34B H 0.1969 0.2273 0.7141 0.040 Uiso 1 1 calc R . .
H34C H 0.1772 0.1682 0.7752 0.040 Uiso 1 1 calc R . .
C35 C 0.34270(17) 0.4080(2) 0.9011(2) 0.0370(9) Uani 1 1 d . . .
H35 H 0.3811 0.3898 0.9549 0.044 Uiso 1 1 d R A .
C36 C 0.28219(15) 0.44106(19) 0.91964(18) 0.0222(6) Uani 1 1 d . A .
H36A H 0.2991 0.4870 0.9606 0.033 Uiso 1 1 calc R . .
H36B H 0.2636 0.3949 0.9419 0.033 Uiso 1 1 calc R . .
H36C H 0.2448 0.4626 0.8684 0.033 Uiso 1 1 calc R . .
C37A C 0.3621(2) 0.4903(3) 0.8538(3) 0.0189(11) Uani 0.630(7) 1 d P A 1
H37A H 0.3187 0.5121 0.8098 0.028 Uiso 0.630(7) 1 calc PR A 1
H37B H 0.3943 0.4716 0.8295 0.028 Uiso 0.630(7) 1 calc PR A 1
H37C H 0.3845 0.5353 0.8944 0.028 Uiso 0.630(7) 1 calc PR A 1
C37B C 0.3988(4) 0.4604(5) 0.9120(5) 0.024(2) Uani 0.370(7) 1 d P A 2
H37D H 0.3862 0.4980 0.8638 0.036 Uiso 0.370(7) 1 calc PR A 2
H37E H 0.4397 0.4259 0.9176 0.036 Uiso 0.370(7) 1 calc PR A 2
H37F H 0.4104 0.4946 0.9622 0.036 Uiso 0.370(7) 1 calc PR A 2
C38 C 0.55023(15) 0.3230(2) 0.68111(19) 0.0271(7) Uani 1 1 d . . .
H38A H 0.5301 0.2989 0.6250 0.041 Uiso 1 1 calc R . .
H38B H 0.5947 0.2942 0.7145 0.041 Uiso 1 1 calc R . .
H38C H 0.5591 0.3837 0.6779 0.041 Uiso 1 1 calc R . .
C39 C 0.21707(16) 0.4082(2) 0.7006(2) 0.0283(7) Uani 1 1 d . . .
H39A H 0.2248 0.4693 0.6989 0.042 Uiso 1 1 calc R . .
H39B H 0.1940 0.3968 0.7380 0.042 Uiso 1 1 calc R . .
H39C H 0.1870 0.3879 0.6447 0.042 Uiso 1 1 calc R . .
C40 C 0.46000(14) 0.26544(17) 0.92919(16) 0.0164(5) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C20 1.915(3) . ?
Mo1 N1 2.275(2) . ?
Mo1 P2 2.3764(7) . ?
Mo1 P1 2.3825(7) . ?
Mo1 I1 2.7657(3) . ?
Mo1 I2 2.8504(3) . ?
Mo2 C40 1.919(3) . ?
Mo2 N4 2.275(2) . ?
Mo2 P3 2.3784(7) . ?
Mo2 P4 2.3841(7) . ?
Mo2 I3 2.7602(3) . ?
Mo2 I4 2.8531(3) . ?
P1 N2 1.705(2) . ?
P1 C6 1.846(3) . ?
P1 C9 1.846(3) . ?
P2 N3 1.708(2) . ?
P2 C12 1.838(3) . ?
P2 C15 1.852(3) . ?
P3 N5 1.704(2) . ?
P3 C26 1.837(3) . ?
P3 C29 1.844(3) . ?
P4 N6 1.706(2) . ?
P4 C32 1.847(3) . ?
P4 C35 1.853(3) . ?
N1 C1 1.360(3) . ?
N1 C5 1.365(3) . ?
N2 C1 1.379(3) . ?
N2 C18 1.473(3) . ?
N3 C5 1.377(3) . ?
N3 C19 1.468(3) . ?
N4 C25 1.359(3) . ?
N4 C21 1.365(3) . ?
N5 C21 1.376(3) . ?
N5 C38 1.477(3) . ?
N6 C25 1.386(3) . ?
N6 C39 1.463(3) . ?
O1 C20 1.168(3) . ?
O2 C40 1.170(3) . ?
C1 C2 1.399(3) . ?
C2 C3 1.375(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.374(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(4) . ?
C4 H4 0.9500 . ?
C6 C8 1.523(4) . ?
C6 C7 1.532(4) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.530(4) . ?
C9 C11 1.534(4) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.529(4) . ?
C12 C13 1.535(4) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.531(4) . ?
C15 C17 1.535(4) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 C22 1.387(4) . ?
C22 C23 1.377(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.378(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.389(4) . ?
C24 H24 0.9500 . ?
C26 C28 1.530(4) . ?
C26 C27 1.534(4) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30A 1.509(5) . ?
C29 C31 1.525(4) . ?
C29 C30B 1.632(8) . ?
C29 H29 0.9998 . ?
C30A H30A 0.9800 . ?
C30A H30B 0.9800 . ?
C30A H30C 0.9800 . ?
C30B H30D 0.9800 . ?
C30B H30E 0.9800 . ?
C30B H30F 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.529(4) . ?
C32 C34 1.535(4) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C37B 1.378(8) . ?
C35 C36 1.518(4) . ?
C35 C37A 1.680(6) . ?
C35 H35 0.9998 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37A H37A 0.9800 . ?
C37A H37B 0.9800 . ?
C37A H37C 0.9800 . ?
C37B H37D 0.9800 . ?
C37B H37E 0.9800 . ?
C37B H37F 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?

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
C20 Mo1 N1 115.13(9) . . ?
C20 Mo1 P2 79.45(8) . . ?
N1 Mo1 P2 70.91(6) . . ?
C20 Mo1 P1 79.90(7) . . ?
N1 Mo1 P1 74.11(6) . . ?
P2 Mo1 P1 126.11(2) . . ?
C20 Mo1 I1 79.32(8) . . ?
N1 Mo1 I1 165.50(5) . . ?
P2 Mo1 I1 115.137(18) . . ?
P1 Mo1 I1 108.984(17) . . ?
C20 Mo1 I2 163.17(7) . . ?
N1 Mo1 I2 79.54(5) . . ?
P2 Mo1 I2 98.990(17) . . ?
P1 Mo1 I2 113.461(17) . . ?
I1 Mo1 I2 86.359(8) . . ?
C40 Mo2 N4 115.12(10) . . ?
C40 Mo2 P3 79.16(8) . . ?
N4 Mo2 P3 72.39(6) . . ?
C40 Mo2 P4 79.89(8) . . ?
N4 Mo2 P4 72.81(6) . . ?
P3 Mo2 P4 126.06(3) . . ?
C40 Mo2 I3 81.22(8) . . ?
N4 Mo2 I3 163.52(5) . . ?
P3 Mo2 I3 110.756(18) . . ?
P4 Mo2 I3 114.275(19) . . ?
C40 Mo2 I4 167.21(8) . . ?
N4 Mo2 I4 77.61(5) . . ?
P3 Mo2 I4 104.813(18) . . ?
P4 Mo2 I4 106.385(18) . . ?
I3 Mo2 I4 86.015(8) . . ?
N2 P1 C6 102.58(11) . . ?
N2 P1 C9 107.59(11) . . ?
C6 P1 C9 103.20(12) . . ?
N2 P1 Mo1 105.53(8) . . ?
C6 P1 Mo1 113.72(9) . . ?
C9 P1 Mo1 122.45(8) . . ?
N3 P2 C12 105.80(12) . . ?
N3 P2 C15 104.50(12) . . ?
C12 P2 C15 105.32(12) . . ?
N3 P2 Mo1 102.69(8) . . ?
C12 P2 Mo1 113.75(9) . . ?
C15 P2 Mo1 123.14(9) . . ?
N5 P3 C26 104.89(12) . . ?
N5 P3 C29 105.74(13) . . ?
C26 P3 C29 103.50(12) . . ?
N5 P3 Mo2 103.51(8) . . ?
C26 P3 Mo2 114.40(9) . . ?
C29 P3 Mo2 123.20(9) . . ?
N6 P4 C32 103.89(12) . . ?
N6 P4 C35 105.13(16) . . ?
C32 P4 C35 104.28(14) . . ?
N6 P4 Mo2 103.71(8) . . ?
C32 P4 Mo2 113.46(9) . . ?
C35 P4 Mo2 124.35(11) . . ?
C1 N1 C5 117.7(2) . . ?
C1 N1 Mo1 121.49(16) . . ?
C5 N1 Mo1 120.13(16) . . ?
C1 N2 C18 117.7(2) . . ?
C1 N2 P1 118.16(17) . . ?
C18 N2 P1 124.12(18) . . ?
C5 N3 C19 118.5(2) . . ?
C5 N3 P2 113.66(17) . . ?
C19 N3 P2 124.15(18) . . ?
C25 N4 C21 117.5(2) . . ?
C25 N4 Mo2 121.07(16) . . ?
C21 N4 Mo2 120.26(17) . . ?
C21 N5 C38 118.0(2) . . ?
C21 N5 P3 115.98(18) . . ?
C38 N5 P3 124.98(19) . . ?
C25 N6 C39 118.2(2) . . ?
C25 N6 P4 116.55(18) . . ?
C39 N6 P4 123.96(19) . . ?
N1 C1 N2 116.6(2) . . ?
N1 C1 C2 121.8(2) . . ?
N2 C1 C2 121.5(2) . . ?
C3 C2 C1 118.3(3) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C4 C3 C2 121.1(2) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 118.1(2) . . ?
C3 C4 H4 121.0 . . ?
C5 C4 H4 121.0 . . ?
N1 C5 N3 115.4(2) . . ?
N1 C5 C4 122.5(2) . . ?
N3 C5 C4 122.1(2) . . ?
C8 C6 C7 111.9(2) . . ?
C8 C6 P1 112.10(19) . . ?
C7 C6 P1 111.55(18) . . ?
C8 C6 H6 107.0 . . ?
C7 C6 H6 107.0 . . ?
P1 C6 H6 107.0 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C11 110.1(2) . . ?
C10 C9 P1 110.30(18) . . ?
C11 C9 P1 116.92(18) . . ?
C10 C9 H9 106.3 . . ?
C11 C9 H9 106.3 . . ?
P1 C9 H9 106.3 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C14 C12 C13 111.4(2) . . ?
C14 C12 P2 113.75(18) . . ?
C13 C12 P2 108.64(18) . . ?
C14 C12 H12 107.6 . . ?
C13 C12 H12 107.6 . . ?
P2 C12 H12 107.6 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C17 109.5(2) . . ?
C16 C15 P2 109.81(18) . . ?
C17 C15 P2 115.06(19) . . ?
C16 C15 H15 107.4 . . ?
C17 C15 H15 107.4 . . ?
P2 C15 H15 107.4 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O1 C20 Mo1 177.0(2) . . ?
N4 C21 N5 115.9(2) . . ?
N4 C21 C22 122.2(2) . . ?
N5 C21 C22 121.9(2) . . ?
C23 C22 C21 118.5(3) . . ?
C23 C22 H22 120.7 . . ?
C21 C22 H22 120.7 . . ?
C22 C23 C24 120.7(3) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C23 C24 C25 118.0(3) . . ?
C23 C24 H24 121.0 . . ?
C25 C24 H24 121.0 . . ?
N4 C25 N6 115.8(2) . . ?
N4 C25 C24 122.8(2) . . ?
N6 C25 C24 121.5(2) . . ?
C28 C26 C27 111.3(2) . . ?
C28 C26 P3 113.49(19) . . ?
C27 C26 P3 110.70(19) . . ?
C28 C26 H26 107.0 . . ?
C27 C26 H26 107.0 . . ?
P3 C26 H26 107.0 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30A C29 C31 114.1(3) . . ?
C31 C29 C30B 99.1(3) . . ?
C30A C29 P3 115.0(2) . . ?
C31 C29 P3 115.6(2) . . ?
C30B C29 P3 101.8(3) . . ?
C30A C29 H29 96.1 . . ?
C31 C29 H29 106.6 . . ?
C30B C29 H29 127.4 . . ?
P3 C29 H29 106.9 . . ?
C29 C30A H30A 109.5 . . ?
C29 C30A H30B 109.5 . . ?
C29 C30A H30C 109.5 . . ?
C29 C30B H30D 109.5 . . ?
C29 C30B H30E 109.5 . . ?
H30D C30B H30E 109.5 . . ?
C29 C30B H30F 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 C34 111.4(2) . . ?
C33 C32 P4 110.3(2) . . ?
C34 C32 P4 112.55(19) . . ?
C33 C32 H32 107.4 . . ?
C34 C32 H32 107.4 . . ?
P4 C32 H32 107.4 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C37B C35 C36 119.7(4) . . ?
C36 C35 C37A 103.5(3) . . ?
C37B C35 P4 118.1(4) . . ?
C36 C35 P4 117.6(2) . . ?
C37A C35 P4 104.9(2) . . ?
C36 C35 H35 107.6 . . ?
P4 C35 H35 107.8 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37A H37A 109.5 . . ?
C35 C37A H37B 109.5 . . ?
C35 C37A H37C 109.5 . . ?
C35 C37B H37D 109.5 . . ?
H35 C37B H37D 150.2 . . ?
C35 C37B H37E 109.5 . . ?
H35 C37B H37E 85.4 . . ?
H37D C37B H37E 109.5 . . ?
C35 C37B H37F 109.5 . . ?
H35 C37B H37F 88.2 . . ?
H37D C37B H37F 109.5 . . ?
H37E C37B H37F 109.5 . . ?
N5 C38 H38A 109.5 . . ?
N5 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
N5 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N6 C39 H39A 109.5 . . ?
N6 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N6 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O2 C40 Mo2 179.4(3) . . ?

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
C20 Mo1 P1 N2 -134.31(11) . . . . ?
N1 Mo1 P1 N2 -14.36(9) . . . . ?
P2 Mo1 P1 N2 -65.41(8) . . . . ?
I1 Mo1 P1 N2 150.78(8) . . . . ?
I2 Mo1 P1 N2 56.42(8) . . . . ?
C20 Mo1 P1 C6 114.04(12) . . . . ?
N1 Mo1 P1 C6 -126.01(11) . . . . ?
P2 Mo1 P1 C6 -177.07(9) . . . . ?
I1 Mo1 P1 C6 39.13(9) . . . . ?
I2 Mo1 P1 C6 -55.23(9) . . . . ?
C20 Mo1 P1 C9 -11.05(13) . . . . ?
N1 Mo1 P1 C9 108.89(12) . . . . ?
P2 Mo1 P1 C9 57.84(11) . . . . ?
I1 Mo1 P1 C9 -85.96(11) . . . . ?
I2 Mo1 P1 C9 179.67(10) . . . . ?
C20 Mo1 P2 N3 153.74(11) . . . . ?
N1 Mo1 P2 N3 32.30(10) . . . . ?
P1 Mo1 P2 N3 84.63(8) . . . . ?
I1 Mo1 P2 N3 -133.46(8) . . . . ?
I2 Mo1 P2 N3 -43.27(8) . . . . ?
C20 Mo1 P2 C12 -92.43(12) . . . . ?
N1 Mo1 P2 C12 146.13(11) . . . . ?
P1 Mo1 P2 C12 -161.54(10) . . . . ?
I1 Mo1 P2 C12 -19.63(10) . . . . ?
I2 Mo1 P2 C12 70.56(10) . . . . ?
C20 Mo1 P2 C15 36.77(13) . . . . ?
N1 Mo1 P2 C15 -84.67(12) . . . . ?
P1 Mo1 P2 C15 -32.34(11) . . . . ?
I1 Mo1 P2 C15 109.57(11) . . . . ?
I2 Mo1 P2 C15 -160.24(11) . . . . ?
C40 Mo2 P3 N5 -147.84(13) . . . . ?
N4 Mo2 P3 N5 -26.89(11) . . . . ?
P4 Mo2 P3 N5 -78.97(10) . . . . ?
I3 Mo2 P3 N5 135.97(9) . . . . ?
I4 Mo2 P3 N5 44.64(10) . . . . ?
C40 Mo2 P3 C26 98.64(13) . . . . ?
N4 Mo2 P3 C26 -140.41(11) . . . . ?
P4 Mo2 P3 C26 167.51(10) . . . . ?
I3 Mo2 P3 C26 22.45(10) . . . . ?
I4 Mo2 P3 C26 -68.89(10) . . . . ?
C40 Mo2 P3 C29 -28.46(14) . . . . ?
N4 Mo2 P3 C29 92.49(13) . . . . ?
P4 Mo2 P3 C29 40.41(12) . . . . ?
I3 Mo2 P3 C29 -104.65(11) . . . . ?
I4 Mo2 P3 C29 164.01(11) . . . . ?
C40 Mo2 P4 N6 145.11(12) . . . . ?
N4 Mo2 P4 N6 24.68(10) . . . . ?
P3 Mo2 P4 N6 76.59(9) . . . . ?
I3 Mo2 P4 N6 -139.39(9) . . . . ?
I4 Mo2 P4 N6 -46.34(9) . . . . ?
C40 Mo2 P4 C32 -102.84(13) . . . . ?
N4 Mo2 P4 C32 136.73(11) . . . . ?
P3 Mo2 P4 C32 -171.37(9) . . . . ?
I3 Mo2 P4 C32 -27.35(10) . . . . ?
I4 Mo2 P4 C32 65.70(10) . . . . ?
C40 Mo2 P4 C35 25.63(18) . . . . ?
N4 Mo2 P4 C35 -94.80(17) . . . . ?
P3 Mo2 P4 C35 -42.89(17) . . . . ?
I3 Mo2 P4 C35 101.13(16) . . . . ?
I4 Mo2 P4 C35 -165.82(16) . . . . ?
C20 Mo1 N1 C1 89.9(2) . . . . ?
P2 Mo1 N1 C1 157.77(19) . . . . ?
P1 Mo1 N1 C1 19.45(17) . . . . ?
I1 Mo1 N1 C1 -85.0(3) . . . . ?
I2 Mo1 N1 C1 -98.81(18) . . . . ?
C20 Mo1 N1 C5 -99.83(19) . . . . ?
P2 Mo1 N1 C5 -31.94(17) . . . . ?
P1 Mo1 N1 C5 -170.27(19) . . . . ?
I1 Mo1 N1 C5 85.2(3) . . . . ?
I2 Mo1 N1 C5 71.47(17) . . . . ?
C6 P1 N2 C1 131.85(19) . . . . ?
C9 P1 N2 C1 -119.71(19) . . . . ?
Mo1 P1 N2 C1 12.5(2) . . . . ?
C6 P1 N2 C18 -48.8(2) . . . . ?
C9 P1 N2 C18 59.6(2) . . . . ?
Mo1 P1 N2 C18 -168.17(19) . . . . ?
C12 P2 N3 C5 -158.40(18) . . . . ?
C15 P2 N3 C5 90.7(2) . . . . ?
Mo1 P2 N3 C5 -38.87(19) . . . . ?
C12 P2 N3 C19 43.5(2) . . . . ?
C15 P2 N3 C19 -67.4(2) . . . . ?
Mo1 P2 N3 C19 163.0(2) . . . . ?
C40 Mo2 N4 C25 -95.8(2) . . . . ?
P3 Mo2 N4 C25 -164.3(2) . . . . ?
P4 Mo2 N4 C25 -26.15(18) . . . . ?
I3 Mo2 N4 C25 92.0(3) . . . . ?
I4 Mo2 N4 C25 85.58(19) . . . . ?
C40 Mo2 N4 C21 96.7(2) . . . . ?
P3 Mo2 N4 C21 28.26(18) . . . . ?
P4 Mo2 N4 C21 166.4(2) . . . . ?
I3 Mo2 N4 C21 -75.5(3) . . . . ?
I4 Mo2 N4 C21 -81.88(18) . . . . ?
C26 P3 N5 C21 151.2(2) . . . . ?
C29 P3 N5 C21 -99.7(2) . . . . ?
Mo2 P3 N5 C21 31.0(2) . . . . ?
C26 P3 N5 C38 -40.5(3) . . . . ?
C29 P3 N5 C38 68.5(3) . . . . ?
Mo2 P3 N5 C38 -160.7(2) . . . . ?
C32 P4 N6 C25 -147.4(2) . . . . ?
C35 P4 N6 C25 103.3(2) . . . . ?
Mo2 P4 N6 C25 -28.5(2) . . . . ?
C32 P4 N6 C39 46.0(3) . . . . ?
C35 P4 N6 C39 -63.3(3) . . . . ?
Mo2 P4 N6 C39 164.9(2) . . . . ?
C5 N1 C1 N2 171.5(2) . . . . ?
Mo1 N1 C1 N2 -17.9(3) . . . . ?
C5 N1 C1 C2 -8.1(3) . . . . ?
Mo1 N1 C1 C2 162.38(19) . . . . ?
C18 N2 C1 N1 -177.5(2) . . . . ?
P1 N2 C1 N1 1.8(3) . . . . ?
C18 N2 C1 C2 2.2(4) . . . . ?
P1 N2 C1 C2 -178.49(19) . . . . ?
N1 C1 C2 C3 3.3(4) . . . . ?
N2 C1 C2 C3 -176.3(2) . . . . ?
C1 C2 C3 C4 2.9(4) . . . . ?
C2 C3 C4 C5 -4.1(4) . . . . ?
C1 N1 C5 N3 -171.7(2) . . . . ?
Mo1 N1 C5 N3 17.6(3) . . . . ?
C1 N1 C5 C4 7.0(4) . . . . ?
Mo1 N1 C5 C4 -163.67(19) . . . . ?
C19 N3 C5 N1 176.2(2) . . . . ?
P2 N3 C5 N1 16.8(3) . . . . ?
C19 N3 C5 C4 -2.6(4) . . . . ?
P2 N3 C5 C4 -162.0(2) . . . . ?
C3 C4 C5 N1 -1.0(4) . . . . ?
C3 C4 C5 N3 177.6(2) . . . . ?
N2 P1 C6 C8 -62.1(2) . . . . ?
C9 P1 C6 C8 -173.9(2) . . . . ?
Mo1 P1 C6 C8 51.3(2) . . . . ?
N2 P1 C6 C7 171.45(18) . . . . ?
C9 P1 C6 C7 59.7(2) . . . . ?
Mo1 P1 C6 C7 -75.13(19) . . . . ?
N2 P1 C9 C10 60.2(2) . . . . ?
C6 P1 C9 C10 168.20(18) . . . . ?
Mo1 P1 C9 C10 -62.1(2) . . . . ?
N2 P1 C9 C11 -66.5(2) . . . . ?
C6 P1 C9 C11 41.5(2) . . . . ?
Mo1 P1 C9 C11 171.18(17) . . . . ?
N3 P2 C12 C14 56.4(2) . . . . ?
C15 P2 C12 C14 166.7(2) . . . . ?
Mo1 P2 C12 C14 -55.6(2) . . . . ?
N3 P2 C12 C13 -178.84(18) . . . . ?
C15 P2 C12 C13 -68.5(2) . . . . ?
Mo1 P2 C12 C13 69.19(19) . . . . ?
N3 P2 C15 C16 -44.8(2) . . . . ?
C12 P2 C15 C16 -156.09(19) . . . . ?
Mo1 P2 C15 C16 71.3(2) . . . . ?
N3 P2 C15 C17 79.2(2) . . . . ?
C12 P2 C15 C17 -32.0(2) . . . . ?
Mo1 P2 C15 C17 -164.66(17) . . . . ?
C25 N4 C21 N5 174.2(2) . . . . ?
Mo2 N4 C21 N5 -17.9(3) . . . . ?
C25 N4 C21 C22 -5.6(4) . . . . ?
Mo2 N4 C21 C22 162.3(2) . . . . ?
C38 N5 C21 N4 179.7(2) . . . . ?
P3 N5 C21 N4 -11.2(3) . . . . ?
C38 N5 C21 C22 -0.6(4) . . . . ?
P3 N5 C21 C22 168.6(2) . . . . ?
N4 C21 C22 C23 2.6(4) . . . . ?
N5 C21 C22 C23 -177.2(3) . . . . ?
C21 C22 C23 C24 1.7(4) . . . . ?
C22 C23 C24 C25 -2.6(4) . . . . ?
C21 N4 C25 N6 -175.6(2) . . . . ?
Mo2 N4 C25 N6 16.6(3) . . . . ?
C21 N4 C25 C24 4.6(4) . . . . ?
Mo2 N4 C25 C24 -163.2(2) . . . . ?
C39 N6 C25 N4 177.8(3) . . . . ?
P4 N6 C25 N4 10.4(3) . . . . ?
C39 N6 C25 C24 -2.4(4) . . . . ?
P4 N6 C25 C24 -169.8(2) . . . . ?
C23 C24 C25 N4 -0.6(4) . . . . ?
C23 C24 C25 N6 179.6(3) . . . . ?
N5 P3 C26 C28 -60.3(2) . . . . ?
C29 P3 C26 C28 -170.9(2) . . . . ?
Mo2 P3 C26 C28 52.4(2) . . . . ?
N5 P3 C26 C27 173.68(19) . . . . ?
C29 P3 C26 C27 63.0(2) . . . . ?
Mo2 P3 C26 C27 -73.6(2) . . . . ?
N5 P3 C29 C30A 69.0(3) . . . . ?
C26 P3 C29 C30A 179.0(3) . . . . ?
Mo2 P3 C29 C30A -49.4(3) . . . . ?
N5 P3 C29 C31 -67.3(2) . . . . ?
C26 P3 C29 C31 42.7(3) . . . . ?
Mo2 P3 C29 C31 174.40(18) . . . . ?
N5 P3 C29 C30B 39.0(3) . . . . ?
C26 P3 C29 C30B 149.0(3) . . . . ?
Mo2 P3 C29 C30B -79.4(3) . . . . ?
N6 P4 C32 C33 -179.5(2) . . . . ?
C35 P4 C32 C33 -69.6(2) . . . . ?
Mo2 P4 C32 C33 68.5(2) . . . . ?
N6 P4 C32 C34 55.4(2) . . . . ?
C35 P4 C32 C34 165.3(2) . . . . ?
Mo2 P4 C32 C34 -56.6(2) . . . . ?
N6 P4 C35 C37B -76.3(5) . . . . ?
C32 P4 C35 C37B 174.7(5) . . . . ?
Mo2 P4 C35 C37B 42.6(6) . . . . ?
N6 P4 C35 C36 79.8(3) . . . . ?
C32 P4 C35 C36 -29.2(3) . . . . ?
Mo2 P4 C35 C36 -161.4(2) . . . . ?
N6 P4 C35 C37A -34.5(2) . . . . ?
C32 P4 C35 C37A -143.5(2) . . . . ?
Mo2 P4 C35 C37A 84.3(3) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.224
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.125
_database_code_depnum_ccdc_archive 'CCDC 1004519'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4-1680

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
4-1680 [Mo(PNPMe-iPr)(CO)Br2], 
Dibromo-carbonyl-[N,N'-bis(diisopropylphosphino)-N,N'-dimethyl-2,6-
diaminopyridine-\kP,N¹,P']-molybdenum(iv)
;
_chemical_name_common            '4-1680 [Mo(PNPMe-iPr)(CO)Br2]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H37 Br2 Mo N3 O P2'
_chemical_formula_sum            'C20 H37 Br2 Mo N3 O P2'
_chemical_formula_weight         653.23

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '
_symmetry_space_group_name_Hall  '-P 2yn   '

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

_cell_length_a                   15.3996(8)
_cell_length_b                   11.2076(5)
_cell_length_c                   15.6189(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.005(2)
_cell_angle_gamma                90.00
_cell_volume                     2603.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9498
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      37.58

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    3.712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.36
_exptl_absorpt_correction_T_max  0.44
_exptl_absorpt_process_details   'program SADABS'

_exptl_special_details           
; 
4-1680 [Mo(PNPMe-iPr)(CO)Br2] is the first of two
polymorphs of the molecular complex [Mo(PNPMe-iPr)(CO)Br2].
The second polymorph, 4b-1702 [Mo(PNPMe-iPr)(CO)Br2],
reported as the 5th crystal structure in this CIF, has 
a higher density of 1.732 g/cm3 (4-1680 has 1.666) and
should be the thermodynamically more stable form.
The crystallization of 4-1680 may be kinetically favoured.
Because 4-1680 [Mo(PNPMe-iPr)(CO)Br2] is isostructural
with 5-1701 [Mo(PNPMe-iPr)(CO)Cl2], the latter complex
might also crystallize in a second polymorphic form 
of higher density.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Kappa APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            54727
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0135
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.16
_diffrn_reflns_theta_max         30.00
_reflns_number_total             7581
_reflns_number_gt                7003
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0242P)²+1.9354P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7581
_refine_ls_number_parameters     272
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0195
_refine_ls_wR_factor_ref         0.0498
_refine_ls_wR_factor_gt          0.0483
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.215876(9) 0.682483(13) 0.453408(10) 0.01051(3) Uani 1 1 d . . .
Br1 Br 0.134084(11) 0.839368(15) 0.343633(10) 0.01950(4) Uani 1 1 d . . .
Br2 Br 0.361930(11) 0.767525(15) 0.417987(12) 0.02036(4) Uani 1 1 d . . .
P1 P 0.20460(2) 0.48406(3) 0.39646(2) 0.01269(7) Uani 1 1 d . . .
P2 P 0.21917(3) 0.74490(3) 0.59866(2) 0.01449(7) Uani 1 1 d . . .
O1 O 0.01926(8) 0.62859(11) 0.45337(8) 0.0235(2) Uani 1 1 d . . .
N1 N 0.32343(8) 0.57100(11) 0.54541(8) 0.0127(2) Uani 1 1 d . . .
N2 N 0.31294(8) 0.43480(11) 0.43086(8) 0.0147(2) Uani 1 1 d . . .
N3 N 0.32278(9) 0.70226(11) 0.66123(8) 0.0160(2) Uani 1 1 d . . .
C1 C 0.35964(9) 0.47531(13) 0.51344(9) 0.0144(3) Uani 1 1 d . . .
C2 C 0.43857(10) 0.42010(14) 0.56098(10) 0.0189(3) Uani 1 1 d . . .
H2 H 0.4637 0.3554 0.5363 0.023 Uiso 1 1 calc R . .
C3 C 0.47922(10) 0.46185(15) 0.64475(11) 0.0207(3) Uani 1 1 d . . .
H3 H 0.5333 0.4260 0.6782 0.025 Uiso 1 1 calc R . .
C4 C 0.44193(10) 0.55531(15) 0.68049(10) 0.0194(3) Uani 1 1 d . . .
H4 H 0.4689 0.5830 0.7388 0.023 Uiso 1 1 calc R . .
C5 C 0.36374(9) 0.60820(13) 0.62901(9) 0.0140(2) Uani 1 1 d . . .
C6 C 0.17690(10) 0.48224(14) 0.27474(9) 0.0176(3) Uani 1 1 d . . .
H6 H 0.1835 0.3984 0.2554 0.021 Uiso 1 1 calc R . .
C7 C 0.07868(12) 0.51990(18) 0.23694(11) 0.0273(4) Uani 1 1 d . . .
H7A H 0.0720 0.6046 0.2495 0.041 Uiso 1 1 calc R . .
H7B H 0.0399 0.4722 0.2645 0.041 Uiso 1 1 calc R . .
H7C H 0.0614 0.5070 0.1727 0.041 Uiso 1 1 calc R . .
C8 C 0.23962(12) 0.56104(15) 0.23860(10) 0.0218(3) Uani 1 1 d . . .
H8A H 0.2252 0.5531 0.1740 0.033 Uiso 1 1 calc R . .
H8B H 0.3020 0.5364 0.2643 0.033 Uiso 1 1 calc R . .
H8C H 0.2321 0.6444 0.2542 0.033 Uiso 1 1 calc R . .
C9 C 0.13565(10) 0.36429(13) 0.42741(10) 0.0175(3) Uani 1 1 d . . .
H9 H 0.0768 0.4004 0.4292 0.021 Uiso 1 1 calc R . .
C10 C 0.18174(12) 0.32072(14) 0.52135(11) 0.0210(3) Uani 1 1 d . . .
H10A H 0.1392 0.2733 0.5442 0.031 Uiso 1 1 calc R . .
H10B H 0.2016 0.3896 0.5601 0.031 Uiso 1 1 calc R . .
H10C H 0.2339 0.2715 0.5197 0.031 Uiso 1 1 calc R . .
C11 C 0.11539(13) 0.25732(16) 0.36430(13) 0.0274(4) Uani 1 1 d . . .
H11A H 0.1719 0.2196 0.3613 0.041 Uiso 1 1 calc R . .
H11B H 0.0828 0.2845 0.3051 0.041 Uiso 1 1 calc R . .
H11C H 0.0785 0.1995 0.3862 0.041 Uiso 1 1 calc R . .
C12 C 0.21772(12) 0.90921(14) 0.60930(11) 0.0228(3) Uani 1 1 d . . .
H12 H 0.2319 0.9279 0.6741 0.027 Uiso 1 1 calc R . .
C13 C 0.12326(14) 0.95814(16) 0.56705(12) 0.0296(4) Uani 1 1 d . . .
H13A H 0.1236 1.0452 0.5733 0.044 Uiso 1 1 calc R . .
H13B H 0.0805 0.9235 0.5968 0.044 Uiso 1 1 calc R . .
H13C H 0.1054 0.9370 0.5040 0.044 Uiso 1 1 calc R . .
C14 C 0.28961(14) 0.96974(16) 0.57288(13) 0.0317(4) Uani 1 1 d . . .
H14A H 0.2724 0.9652 0.5080 0.047 Uiso 1 1 calc R . .
H14B H 0.3473 0.9293 0.5960 0.047 Uiso 1 1 calc R . .
H14C H 0.2952 1.0536 0.5913 0.047 Uiso 1 1 calc R . .
C15 C 0.13760(11) 0.69557(14) 0.65974(10) 0.0186(3) Uani 1 1 d . . .
H15 H 0.0763 0.7156 0.6220 0.022 Uiso 1 1 calc R . .
C16 C 0.14214(12) 0.55975(14) 0.66902(11) 0.0221(3) Uani 1 1 d . . .
H16A H 0.2037 0.5358 0.6991 0.033 Uiso 1 1 calc R . .
H16B H 0.1245 0.5231 0.6101 0.033 Uiso 1 1 calc R . .
H16C H 0.1011 0.5333 0.7039 0.033 Uiso 1 1 calc R . .
C17 C 0.14653(14) 0.75455(17) 0.75026(11) 0.0286(4) Uani 1 1 d . . .
H17A H 0.0967 0.7290 0.7742 0.043 Uiso 1 1 calc R . .
H17B H 0.1450 0.8415 0.7434 0.043 Uiso 1 1 calc R . .
H17C H 0.2037 0.7308 0.7910 0.043 Uiso 1 1 calc R . .
C18 C 0.34752(11) 0.33074(14) 0.39331(11) 0.0200(3) Uani 1 1 d . . .
H18A H 0.4100 0.3453 0.3924 0.030 Uiso 1 1 calc R . .
H18B H 0.3109 0.3170 0.3327 0.030 Uiso 1 1 calc R . .
H18C H 0.3447 0.2603 0.4297 0.030 Uiso 1 1 calc R . .
C19 C 0.36703(12) 0.74854(16) 0.74960(11) 0.0248(3) Uani 1 1 d . . .
H19A H 0.3668 0.6871 0.7942 0.037 Uiso 1 1 calc R . .
H19B H 0.3347 0.8191 0.7619 0.037 Uiso 1 1 calc R . .
H19C H 0.4292 0.7703 0.7518 0.037 Uiso 1 1 calc R . .
C20 C 0.09468(10) 0.64536(13) 0.45554(9) 0.0160(3) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C20 1.9209(15) . ?
Mo1 N1 2.2665(12) . ?
Mo1 P2 2.3620(4) . ?
Mo1 P1 2.3847(4) . ?
Mo1 Br1 2.5494(2) . ?
Mo1 Br2 2.6301(3) . ?
P1 N2 1.7068(13) . ?
P1 C6 1.8375(15) . ?
P1 C9 1.8517(15) . ?
P2 N3 1.7093(13) . ?
P2 C15 1.8478(16) . ?
P2 C12 1.8497(16) . ?
O1 C20 1.1684(19) . ?
N1 C5 1.3581(18) . ?
N1 C1 1.3618(18) . ?
N2 C1 1.3807(19) . ?
N2 C18 1.4661(19) . ?
N3 C5 1.3881(19) . ?
N3 C19 1.4669(19) . ?
C1 C2 1.394(2) . ?
C2 C3 1.378(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.380(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.395(2) . ?
C4 H4 0.9500 . ?
C6 C8 1.521(2) . ?
C6 C7 1.534(2) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C11 1.532(2) . ?
C9 C10 1.535(2) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.528(3) . ?
C12 C13 1.535(3) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.529(2) . ?
C15 C17 1.534(2) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

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
C20 Mo1 N1 115.05(5) . . ?
C20 Mo1 P2 80.03(4) . . ?
N1 Mo1 P2 73.97(3) . . ?
C20 Mo1 P1 80.05(4) . . ?
N1 Mo1 P1 72.13(3) . . ?
P2 Mo1 P1 128.010(15) . . ?
C20 Mo1 Br1 81.26(4) . . ?
N1 Mo1 Br1 163.60(3) . . ?
P2 Mo1 Br1 109.009(11) . . ?
P1 Mo1 Br1 114.628(11) . . ?
C20 Mo1 Br2 165.88(4) . . ?
N1 Mo1 Br2 78.98(3) . . ?
P2 Mo1 Br2 106.728(11) . . ?
P1 Mo1 Br2 104.073(11) . . ?
Br1 Mo1 Br2 84.785(8) . . ?
N2 P1 C6 105.56(6) . . ?
N2 P1 C9 105.26(7) . . ?
C6 P1 C9 105.48(7) . . ?
N2 P1 Mo1 102.32(5) . . ?
C6 P1 Mo1 111.79(5) . . ?
C9 P1 Mo1 124.75(5) . . ?
N3 P2 C15 106.26(7) . . ?
N3 P2 C12 104.96(7) . . ?
C15 P2 C12 103.05(8) . . ?
N3 P2 Mo1 104.54(5) . . ?
C15 P2 Mo1 123.98(5) . . ?
C12 P2 Mo1 112.54(5) . . ?
C5 N1 C1 117.75(12) . . ?
C5 N1 Mo1 121.16(9) . . ?
C1 N1 Mo1 120.20(9) . . ?
C1 N2 C18 118.68(12) . . ?
C1 N2 P1 114.71(10) . . ?
C18 N2 P1 123.92(11) . . ?
C5 N3 C19 117.76(13) . . ?
C5 N3 P2 116.72(10) . . ?
C19 N3 P2 125.21(11) . . ?
N1 C1 N2 115.96(12) . . ?
N1 C1 C2 122.51(13) . . ?
N2 C1 C2 121.53(13) . . ?
C3 C2 C1 118.30(14) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C4 120.50(14) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C5 118.47(14) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
N1 C5 N3 116.37(12) . . ?
N1 C5 C4 122.36(14) . . ?
N3 C5 C4 121.27(13) . . ?
C8 C6 C7 110.79(14) . . ?
C8 C6 P1 112.20(11) . . ?
C7 C6 P1 109.69(10) . . ?
C8 C6 H6 108.0 . . ?
C7 C6 H6 108.0 . . ?
P1 C6 H6 108.0 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C11 C9 C10 109.44(14) . . ?
C11 C9 P1 115.74(11) . . ?
C10 C9 P1 109.01(11) . . ?
C11 C9 H9 107.4 . . ?
C10 C9 H9 107.4 . . ?
P1 C9 H9 107.4 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C14 C12 C13 112.25(15) . . ?
C14 C12 P2 112.44(12) . . ?
C13 C12 P2 110.44(12) . . ?
C14 C12 H12 107.1 . . ?
C13 C12 H12 107.1 . . ?
P2 C12 H12 107.1 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C17 110.52(14) . . ?
C16 C15 P2 109.04(11) . . ?
C17 C15 P2 115.85(12) . . ?
C16 C15 H15 107.0 . . ?
C17 C15 H15 107.0 . . ?
P2 C15 H15 107.0 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O1 C20 Mo1 175.85(14) . . ?

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
C20 Mo1 P1 N2 -150.36(6) . . . . ?
N1 Mo1 P1 N2 -29.81(5) . . . . ?
P2 Mo1 P1 N2 -81.47(5) . . . . ?
Br1 Mo1 P1 N2 134.13(4) . . . . ?
Br2 Mo1 P1 N2 43.45(4) . . . . ?
C20 Mo1 P1 C6 97.12(7) . . . . ?
N1 Mo1 P1 C6 -142.33(6) . . . . ?
P2 Mo1 P1 C6 166.00(5) . . . . ?
Br1 Mo1 P1 C6 21.61(6) . . . . ?
Br2 Mo1 P1 C6 -69.07(5) . . . . ?
C20 Mo1 P1 C9 -31.71(8) . . . . ?
N1 Mo1 P1 C9 88.83(7) . . . . ?
P2 Mo1 P1 C9 37.17(7) . . . . ?
Br1 Mo1 P1 C9 -107.23(6) . . . . ?
Br2 Mo1 P1 C9 162.10(6) . . . . ?
C20 Mo1 P2 N3 140.95(7) . . . . ?
N1 Mo1 P2 N3 21.09(6) . . . . ?
P1 Mo1 P2 N3 72.05(5) . . . . ?
Br1 Mo1 P2 N3 -141.98(5) . . . . ?
Br2 Mo1 P2 N3 -51.80(5) . . . . ?
C20 Mo1 P2 C15 19.38(8) . . . . ?
N1 Mo1 P2 C15 -100.48(7) . . . . ?
P1 Mo1 P2 C15 -49.52(7) . . . . ?
Br1 Mo1 P2 C15 96.44(6) . . . . ?
Br2 Mo1 P2 C15 -173.38(6) . . . . ?
C20 Mo1 P2 C12 -105.70(8) . . . . ?
N1 Mo1 P2 C12 134.45(7) . . . . ?
P1 Mo1 P2 C12 -174.59(6) . . . . ?
Br1 Mo1 P2 C12 -28.63(6) . . . . ?
Br2 Mo1 P2 C12 61.55(6) . . . . ?
C20 Mo1 N1 C5 -92.59(11) . . . . ?
P2 Mo1 N1 C5 -22.05(10) . . . . ?
P1 Mo1 N1 C5 -162.04(11) . . . . ?
Br1 Mo1 N1 C5 80.90(15) . . . . ?
Br2 Mo1 N1 C5 89.11(10) . . . . ?
C20 Mo1 N1 C1 98.43(11) . . . . ?
P2 Mo1 N1 C1 168.97(11) . . . . ?
P1 Mo1 N1 C1 28.98(10) . . . . ?
Br1 Mo1 N1 C1 -88.08(15) . . . . ?
Br2 Mo1 N1 C1 -79.87(10) . . . . ?
C6 P1 N2 C1 153.49(11) . . . . ?
C9 P1 N2 C1 -95.21(11) . . . . ?
Mo1 P1 N2 C1 36.41(11) . . . . ?
C6 P1 N2 C18 -45.40(13) . . . . ?
C9 P1 N2 C18 65.89(13) . . . . ?
Mo1 P1 N2 C18 -162.48(11) . . . . ?
C15 P2 N3 C5 108.18(11) . . . . ?
C12 P2 N3 C5 -143.07(11) . . . . ?
Mo1 P2 N3 C5 -24.43(11) . . . . ?
C15 P2 N3 C19 -65.19(14) . . . . ?
C12 P2 N3 C19 43.56(15) . . . . ?
Mo1 P2 N3 C19 162.20(12) . . . . ?
C5 N1 C1 N2 175.36(12) . . . . ?
Mo1 N1 C1 N2 -15.29(16) . . . . ?
C5 N1 C1 C2 -4.0(2) . . . . ?
Mo1 N1 C1 C2 165.33(11) . . . . ?
C18 N2 C1 N1 -178.95(12) . . . . ?
P1 N2 C1 N1 -16.79(16) . . . . ?
C18 N2 C1 C2 0.4(2) . . . . ?
P1 N2 C1 C2 162.60(11) . . . . ?
N1 C1 C2 C3 2.4(2) . . . . ?
N2 C1 C2 C3 -176.94(14) . . . . ?
C1 C2 C3 C4 0.5(2) . . . . ?
C2 C3 C4 C5 -1.7(2) . . . . ?
C1 N1 C5 N3 -177.02(12) . . . . ?
Mo1 N1 C5 N3 13.74(16) . . . . ?
C1 N1 C5 C4 2.8(2) . . . . ?
Mo1 N1 C5 C4 -166.44(11) . . . . ?
C19 N3 C5 N1 -177.02(13) . . . . ?
P2 N3 C5 N1 9.10(17) . . . . ?
C19 N3 C5 C4 3.2(2) . . . . ?
P2 N3 C5 C4 -170.72(11) . . . . ?
C3 C4 C5 N1 0.0(2) . . . . ?
C3 C4 C5 N3 179.78(14) . . . . ?
N2 P1 C6 C8 -58.98(12) . . . . ?
C9 P1 C6 C8 -170.12(11) . . . . ?
Mo1 P1 C6 C8 51.50(12) . . . . ?
N2 P1 C6 C7 177.43(12) . . . . ?
C9 P1 C6 C7 66.29(13) . . . . ?
Mo1 P1 C6 C7 -72.10(12) . . . . ?
N2 P1 C9 C11 -80.38(13) . . . . ?
C6 P1 C9 C11 30.97(14) . . . . ?
Mo1 P1 C9 C11 162.34(10) . . . . ?
N2 P1 C9 C10 43.47(12) . . . . ?
C6 P1 C9 C10 154.82(10) . . . . ?
Mo1 P1 C9 C10 -73.82(11) . . . . ?
N3 P2 C12 C14 61.90(13) . . . . ?
C15 P2 C12 C14 172.97(12) . . . . ?
Mo1 P2 C12 C14 -51.20(14) . . . . ?
N3 P2 C12 C13 -171.86(11) . . . . ?
C15 P2 C12 C13 -60.79(13) . . . . ?
Mo1 P2 C12 C13 75.05(12) . . . . ?
N3 P2 C15 C16 -61.22(12) . . . . ?
C12 P2 C15 C16 -171.32(11) . . . . ?
Mo1 P2 C15 C16 59.57(13) . . . . ?
N3 P2 C15 C17 64.19(14) . . . . ?
C12 P2 C15 C17 -45.91(14) . . . . ?
Mo1 P2 C15 C17 -175.02(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.149
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.069
_database_code_depnum_ccdc_archive 'CCDC 1004520'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5-1701

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
5-1701 [Mo(PNPMe-iPr)(CO)Cl2], 
Diiodo-carbonyl-[N,N'-bis(diisopropylphosphino)-N,N'-dimethyl-2,6-
diaminopyridine-\kP,N¹,P']-molybdenum(iv)
;
_chemical_name_common            '5-1701 [Mo(PNPMe-iPr)(CO)Cl2]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H37 Cl2 Mo N3 O P2'
_chemical_formula_sum            'C20 H37 Cl2 Mo N3 O P2'
_chemical_formula_weight         564.31

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '

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

_cell_length_a                   15.2750(3)
_cell_length_b                   11.3110(2)
_cell_length_c                   15.3045(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.401(1)
_cell_angle_gamma                90.00
_cell_volume                     2536.65(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9970
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      30.10

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1168
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
; 
The compound is isostructural with the corresponding Br-compound.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            39490
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0115
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         30.00
_reflns_number_total             7384
_reflns_number_gt                7091
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0217P)²+1.2475P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7384
_refine_ls_number_parameters     272
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0169
_refine_ls_wR_factor_ref         0.0453
_refine_ls_wR_factor_gt          0.0447
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.217098(5) 0.673859(7) 0.447416(5) 0.00902(3) Uani 1 1 d . . .
Cl1 Cl 0.138985(17) 0.81839(2) 0.337687(17) 0.01785(5) Uani 1 1 d . . .
Cl2 Cl 0.355205(16) 0.75116(2) 0.412226(18) 0.01805(5) Uani 1 1 d . . .
P1 P 0.203479(16) 0.47645(2) 0.391680(16) 0.01012(5) Uani 1 1 d . . .
P2 P 0.224944(17) 0.73945(2) 0.595678(16) 0.01113(5) Uani 1 1 d . . .
O1 O 0.01858(5) 0.62444(7) 0.44872(5) 0.01908(15) Uani 1 1 d . . .
N1 N 0.32731(5) 0.56426(7) 0.54395(5) 0.01041(14) Uani 1 1 d . . .
N2 N 0.31301(5) 0.42584(7) 0.42836(6) 0.01213(14) Uani 1 1 d . . .
N3 N 0.33056(6) 0.69758(8) 0.66094(6) 0.01323(15) Uani 1 1 d . . .
C1 C 0.36288(6) 0.46805(8) 0.51249(6) 0.01148(16) Uani 1 1 d . . .
C2 C 0.44352(7) 0.41340(9) 0.56190(7) 0.01529(18) Uani 1 1 d . . .
H2 H 0.4678 0.3480 0.5374 0.018 Uiso 1 1 calc R . .
C3 C 0.48705(7) 0.45702(9) 0.64732(7) 0.01705(19) Uani 1 1 d . . .
H3 H 0.5425 0.4219 0.6820 0.020 Uiso 1 1 calc R . .
C4 C 0.45078(7) 0.55133(9) 0.68296(7) 0.01585(18) Uani 1 1 d . . .
H4 H 0.4797 0.5801 0.7424 0.019 Uiso 1 1 calc R . .
C5 C 0.37062(6) 0.60313(8) 0.62934(6) 0.01181(16) Uani 1 1 d . . .
C6 C 0.17397(7) 0.47287(9) 0.26685(6) 0.01438(17) Uani 1 1 d . . .
H6 H 0.1783 0.3891 0.2477 0.017 Uiso 1 1 calc R . .
C7 C 0.07512(8) 0.51423(12) 0.22603(7) 0.0233(2) Uani 1 1 d . . .
H7A H 0.0705 0.5985 0.2389 0.035 Uiso 1 1 calc R . .
H7B H 0.0347 0.4690 0.2532 0.035 Uiso 1 1 calc R . .
H7C H 0.0571 0.5016 0.1600 0.035 Uiso 1 1 calc R . .
C8 C 0.23975(8) 0.54682(10) 0.23075(7) 0.01795(19) Uani 1 1 d . . .
H8A H 0.2225 0.5417 0.1641 0.027 Uiso 1 1 calc R . .
H8B H 0.3020 0.5168 0.2558 0.027 Uiso 1 1 calc R . .
H8C H 0.2370 0.6294 0.2491 0.027 Uiso 1 1 calc R . .
C9 C 0.13257(7) 0.36039(9) 0.42345(7) 0.01420(17) Uani 1 1 d . . .
H9 H 0.0737 0.3980 0.4248 0.017 Uiso 1 1 calc R . .
C10 C 0.18033(8) 0.31735(9) 0.52023(7) 0.01799(19) Uani 1 1 d . . .
H10A H 0.1372 0.2719 0.5436 0.027 Uiso 1 1 calc R . .
H10B H 0.2021 0.3856 0.5599 0.027 Uiso 1 1 calc R . .
H10C H 0.2322 0.2671 0.5191 0.027 Uiso 1 1 calc R . .
C11 C 0.10922(8) 0.25409(10) 0.35868(8) 0.0219(2) Uani 1 1 d . . .
H11A H 0.1656 0.2146 0.3564 0.033 Uiso 1 1 calc R . .
H11B H 0.0760 0.2814 0.2975 0.033 Uiso 1 1 calc R . .
H11C H 0.0711 0.1984 0.3807 0.033 Uiso 1 1 calc R . .
C12 C 0.22519(8) 0.90257(9) 0.60257(7) 0.0187(2) Uani 1 1 d . . .
H12 H 0.2399 0.9241 0.6685 0.022 Uiso 1 1 calc R . .
C13 C 0.12972(9) 0.95191(11) 0.55559(9) 0.0272(2) Uani 1 1 d . . .
H13A H 0.1312 1.0384 0.5591 0.041 Uiso 1 1 calc R . .
H13B H 0.0860 0.9214 0.5861 0.041 Uiso 1 1 calc R . .
H13C H 0.1112 0.9274 0.4916 0.041 Uiso 1 1 calc R . .
C14 C 0.29852(10) 0.95852(11) 0.56532(9) 0.0270(2) Uani 1 1 d . . .
H14A H 0.2823 0.9474 0.4992 0.040 Uiso 1 1 calc R . .
H14B H 0.3575 0.9208 0.5936 0.040 Uiso 1 1 calc R . .
H14C H 0.3028 1.0432 0.5793 0.040 Uiso 1 1 calc R . .
C15 C 0.14357(7) 0.69529(9) 0.65901(7) 0.01485(17) Uani 1 1 d . . .
H15 H 0.0811 0.7148 0.6195 0.018 Uiso 1 1 calc R . .
C16 C 0.14731(8) 0.56126(10) 0.67165(8) 0.0195(2) Uani 1 1 d . . .
H16A H 0.2103 0.5370 0.7015 0.029 Uiso 1 1 calc R . .
H16B H 0.1260 0.5227 0.6121 0.029 Uiso 1 1 calc R . .
H16C H 0.1081 0.5381 0.7096 0.029 Uiso 1 1 calc R . .
C17 C 0.15458(9) 0.75743(12) 0.75057(8) 0.0251(2) Uani 1 1 d . . .
H17A H 0.1053 0.7327 0.7760 0.038 Uiso 1 1 calc R . .
H17B H 0.1519 0.8432 0.7414 0.038 Uiso 1 1 calc R . .
H17C H 0.2136 0.7360 0.7929 0.038 Uiso 1 1 calc R . .
C18 C 0.34620(7) 0.32081(9) 0.39153(7) 0.01666(19) Uani 1 1 d . . .
H18A H 0.4089 0.3345 0.3892 0.025 Uiso 1 1 calc R . .
H18B H 0.3069 0.3050 0.3300 0.025 Uiso 1 1 calc R . .
H18C H 0.3450 0.2527 0.4308 0.025 Uiso 1 1 calc R . .
C19 C 0.37712(8) 0.74520(10) 0.75121(7) 0.0199(2) Uani 1 1 d . . .
H19A H 0.3787 0.6849 0.7976 0.030 Uiso 1 1 calc R . .
H19B H 0.3441 0.8149 0.7632 0.030 Uiso 1 1 calc R . .
H19C H 0.4396 0.7677 0.7532 0.030 Uiso 1 1 calc R . .
C20 C 0.09492(7) 0.63930(9) 0.45060(6) 0.01288(16) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C20 1.9208(10) . ?
Mo1 N1 2.2691(8) . ?
Mo1 P2 2.3579(3) . ?
Mo1 P1 2.3783(3) . ?
Mo1 Cl1 2.4052(2) . ?
Mo1 Cl2 2.4792(3) . ?
P1 N2 1.7064(8) . ?
P1 C6 1.8353(10) . ?
P1 C9 1.8521(10) . ?
P2 N3 1.7072(9) . ?
P2 C15 1.8478(10) . ?
P2 C12 1.8480(11) . ?
O1 C20 1.1704(12) . ?
N1 C5 1.3604(12) . ?
N1 C1 1.3635(12) . ?
N2 C1 1.3827(12) . ?
N2 C18 1.4655(12) . ?
N3 C5 1.3844(13) . ?
N3 C19 1.4662(13) . ?
C1 C2 1.3948(13) . ?
C2 C3 1.3797(15) . ?
C2 H2 0.9500 . ?
C3 C4 1.3832(15) . ?
C3 H3 0.9500 . ?
C4 C5 1.3959(13) . ?
C4 H4 0.9500 . ?
C6 C8 1.5257(14) . ?
C6 C7 1.5351(14) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.5339(15) . ?
C9 C11 1.5350(14) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.5300(17) . ?
C12 C13 1.5372(16) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.5273(15) . ?
C15 C17 1.5339(15) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

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
C20 Mo1 N1 114.82(4) . . ?
C20 Mo1 P2 79.94(3) . . ?
N1 Mo1 P2 73.65(2) . . ?
C20 Mo1 P1 80.26(3) . . ?
N1 Mo1 P1 72.20(2) . . ?
P2 Mo1 P1 128.029(9) . . ?
C20 Mo1 Cl1 82.07(3) . . ?
N1 Mo1 Cl1 163.04(2) . . ?
P2 Mo1 Cl1 109.783(9) . . ?
P1 Mo1 Cl1 114.318(9) . . ?
C20 Mo1 Cl2 165.87(3) . . ?
N1 Mo1 Cl2 79.27(2) . . ?
P2 Mo1 Cl2 106.435(9) . . ?
P1 Mo1 Cl2 104.289(9) . . ?
Cl1 Mo1 Cl2 83.882(9) . . ?
N2 P1 C6 105.36(4) . . ?
N2 P1 C9 105.52(4) . . ?
C6 P1 C9 105.53(5) . . ?
N2 P1 Mo1 102.63(3) . . ?
C6 P1 Mo1 111.40(3) . . ?
C9 P1 Mo1 124.73(3) . . ?
N3 P2 C15 106.42(5) . . ?
N3 P2 C12 104.90(5) . . ?
C15 P2 C12 103.34(5) . . ?
N3 P2 Mo1 104.99(3) . . ?
C15 P2 Mo1 124.11(3) . . ?
C12 P2 Mo1 111.58(3) . . ?
C5 N1 C1 117.58(8) . . ?
C5 N1 Mo1 121.27(6) . . ?
C1 N1 Mo1 120.16(6) . . ?
C1 N2 C18 118.59(8) . . ?
C1 N2 P1 114.94(6) . . ?
C18 N2 P1 123.99(7) . . ?
C5 N3 C19 117.90(8) . . ?
C5 N3 P2 116.59(6) . . ?
C19 N3 P2 125.19(7) . . ?
N1 C1 N2 115.77(8) . . ?
N1 C1 C2 122.77(9) . . ?
N2 C1 C2 121.46(9) . . ?
C3 C2 C1 118.09(9) . . ?
C3 C2 H2 121.0 . . ?
C1 C2 H2 121.0 . . ?
C2 C3 C4 120.66(9) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C3 C4 C5 118.32(9) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
N1 C5 N3 116.23(8) . . ?
N1 C5 C4 122.48(9) . . ?
N3 C5 C4 121.29(9) . . ?
C8 C6 C7 111.00(9) . . ?
C8 C6 P1 111.82(7) . . ?
C7 C6 P1 109.95(7) . . ?
C8 C6 H6 108.0 . . ?
C7 C6 H6 108.0 . . ?
P1 C6 H6 108.0 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C11 109.60(9) . . ?
C10 C9 P1 108.93(7) . . ?
C11 C9 P1 115.60(7) . . ?
C10 C9 H9 107.5 . . ?
C11 C9 H9 107.5 . . ?
P1 C9 H9 107.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C14 C12 C13 111.91(10) . . ?
C14 C12 P2 112.43(8) . . ?
C13 C12 P2 110.45(8) . . ?
C14 C12 H12 107.2 . . ?
C13 C12 H12 107.2 . . ?
P2 C12 H12 107.2 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C17 110.40(9) . . ?
C16 C15 P2 109.15(7) . . ?
C17 C15 P2 116.03(8) . . ?
C16 C15 H15 106.9 . . ?
C17 C15 H15 106.9 . . ?
P2 C15 H15 106.9 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O1 C20 Mo1 175.56(9) . . ?

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
C20 Mo1 P1 N2 -149.63(4) . . . . ?
N1 Mo1 P1 N2 -29.47(4) . . . . ?
P2 Mo1 P1 N2 -80.68(3) . . . . ?
Cl1 Mo1 P1 N2 133.73(3) . . . . ?
Cl2 Mo1 P1 N2 44.05(3) . . . . ?
C20 Mo1 P1 C6 98.07(5) . . . . ?
N1 Mo1 P1 C6 -141.76(4) . . . . ?
P2 Mo1 P1 C6 167.02(3) . . . . ?
Cl1 Mo1 P1 C6 21.44(4) . . . . ?
Cl2 Mo1 P1 C6 -68.24(4) . . . . ?
C20 Mo1 P1 C9 -30.36(5) . . . . ?
N1 Mo1 P1 C9 89.81(5) . . . . ?
P2 Mo1 P1 C9 38.59(4) . . . . ?
Cl1 Mo1 P1 C9 -106.99(4) . . . . ?
Cl2 Mo1 P1 C9 163.33(4) . . . . ?
C20 Mo1 P2 N3 140.91(4) . . . . ?
N1 Mo1 P2 N3 21.16(4) . . . . ?
P1 Mo1 P2 N3 71.82(3) . . . . ?
Cl1 Mo1 P2 N3 -141.37(3) . . . . ?
Cl2 Mo1 P2 N3 -52.05(3) . . . . ?
C20 Mo1 P2 C15 18.59(5) . . . . ?
N1 Mo1 P2 C15 -101.17(5) . . . . ?
P1 Mo1 P2 C15 -50.51(4) . . . . ?
Cl1 Mo1 P2 C15 96.31(4) . . . . ?
Cl2 Mo1 P2 C15 -174.38(4) . . . . ?
C20 Mo1 P2 C12 -105.99(5) . . . . ?
N1 Mo1 P2 C12 134.25(5) . . . . ?
P1 Mo1 P2 C12 -175.09(4) . . . . ?
Cl1 Mo1 P2 C12 -28.27(4) . . . . ?
Cl2 Mo1 P2 C12 61.04(4) . . . . ?
C20 Mo1 N1 C5 -92.66(8) . . . . ?
P2 Mo1 N1 C5 -22.30(6) . . . . ?
P1 Mo1 N1 C5 -162.52(7) . . . . ?
Cl1 Mo1 N1 C5 82.02(10) . . . . ?
Cl2 Mo1 N1 C5 88.53(7) . . . . ?
C20 Mo1 N1 C1 98.98(7) . . . . ?
P2 Mo1 N1 C1 169.34(7) . . . . ?
P1 Mo1 N1 C1 29.12(6) . . . . ?
Cl1 Mo1 N1 C1 -86.34(10) . . . . ?
Cl2 Mo1 N1 C1 -79.83(7) . . . . ?
C6 P1 N2 C1 152.28(7) . . . . ?
C9 P1 N2 C1 -96.35(7) . . . . ?
Mo1 P1 N2 C1 35.57(7) . . . . ?
C6 P1 N2 C18 -45.91(9) . . . . ?
C9 P1 N2 C18 65.47(9) . . . . ?
Mo1 P1 N2 C18 -162.61(7) . . . . ?
C15 P2 N3 C5 108.86(8) . . . . ?
C12 P2 N3 C5 -142.03(7) . . . . ?
Mo1 P2 N3 C5 -24.31(8) . . . . ?
C15 P2 N3 C19 -64.41(10) . . . . ?
C12 P2 N3 C19 44.70(10) . . . . ?
Mo1 P2 N3 C19 162.43(8) . . . . ?
C5 N1 C1 N2 175.20(8) . . . . ?
Mo1 N1 C1 N2 -16.02(11) . . . . ?
C5 N1 C1 C2 -3.71(13) . . . . ?
Mo1 N1 C1 C2 165.07(7) . . . . ?
C18 N2 C1 N1 -178.50(8) . . . . ?
P1 N2 C1 N1 -15.64(11) . . . . ?
C18 N2 C1 C2 0.43(14) . . . . ?
P1 N2 C1 C2 163.29(8) . . . . ?
N1 C1 C2 C3 2.06(15) . . . . ?
N2 C1 C2 C3 -176.79(9) . . . . ?
C1 C2 C3 C4 0.78(15) . . . . ?
C2 C3 C4 C5 -1.78(15) . . . . ?
C1 N1 C5 N3 -177.16(8) . . . . ?
Mo1 N1 C5 N3 14.19(11) . . . . ?
C1 N1 C5 C4 2.63(13) . . . . ?
Mo1 N1 C5 C4 -166.02(7) . . . . ?
C19 N3 C5 N1 -177.58(9) . . . . ?
P2 N3 C5 N1 8.65(11) . . . . ?
C19 N3 C5 C4 2.63(14) . . . . ?
P2 N3 C5 C4 -171.14(8) . . . . ?
C3 C4 C5 N1 0.04(15) . . . . ?
C3 C4 C5 N3 179.82(9) . . . . ?
N2 P1 C6 C8 -57.56(8) . . . . ?
C9 P1 C6 C8 -168.93(7) . . . . ?
Mo1 P1 C6 C8 53.00(8) . . . . ?
N2 P1 C6 C7 178.67(8) . . . . ?
C9 P1 C6 C7 67.30(8) . . . . ?
Mo1 P1 C6 C7 -70.77(8) . . . . ?
N2 P1 C9 C10 43.06(8) . . . . ?
C6 P1 C9 C10 154.32(7) . . . . ?
Mo1 P1 C9 C10 -74.88(7) . . . . ?
N2 P1 C9 C11 -80.83(8) . . . . ?
C6 P1 C9 C11 30.43(9) . . . . ?
Mo1 P1 C9 C11 161.23(6) . . . . ?
N3 P2 C12 C14 60.80(9) . . . . ?
C15 P2 C12 C14 172.13(8) . . . . ?
Mo1 P2 C12 C14 -52.34(9) . . . . ?
N3 P2 C12 C13 -173.41(8) . . . . ?
C15 P2 C12 C13 -62.08(9) . . . . ?
Mo1 P2 C12 C13 73.45(8) . . . . ?
N3 P2 C15 C16 -61.12(8) . . . . ?
C12 P2 C15 C16 -171.33(7) . . . . ?
Mo1 P2 C15 C16 60.56(8) . . . . ?
N3 P2 C15 C17 64.34(9) . . . . ?
C12 P2 C15 C17 -45.87(9) . . . . ?
Mo1 P2 C15 C17 -173.97(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.054
_database_code_depnum_ccdc_archive 'CCDC 1004521'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_8-1703

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
8-1703 [Mo(PNPMe-iPr)(CO)(THF)Cl]SbF6, 
Chloro-carbonyl-tetrahydrofuran-[N,N'-bis(diisopropylphosphino)-N,N'-
dimethyl-2,6-diaminopyridine-\kP,N¹,P']-molybdenum(iv) hexafluoroantimonate.
;
_chemical_name_common            '8-1703 [Mo(PNPMe-iPr)(CO)(THF)Cl]SbF6'
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H45 Cl Mo N3 O2 P2, F6 Sb '
_chemical_formula_sum            'C24 H45 Cl F6 Mo N3 O2 P2 Sb'
_chemical_formula_weight         836.71

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c   '
_symmetry_space_group_name_Hall  '-P 2ybc   '

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

_cell_length_a                   11.4932(4)
_cell_length_b                   9.6174(3)
_cell_length_c                   29.2482(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.387(2)
_cell_angle_gamma                90.00
_cell_volume                     3230.14(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9718
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      30.11

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1680
_exptl_absorpt_coefficient_mu    1.468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            80030
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0136
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         30.00
_reflns_number_total             9421
_reflns_number_gt                8736
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0290P)²+11.2216P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9421
_refine_ls_number_parameters     383
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_ref         0.1027
_refine_ls_wR_factor_gt          0.0998
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_restrained_S_all      1.156
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.73974(8) 0.09558(3) 0.09441(3) 0.01717(17) Uani 1 1 d . . .
Cl1 Cl 0.80640(8) -0.11901(8) 0.06309(3) 0.0389(2) Uani 1 1 d . . .
P1 P 0.55272(6) 0.06350(8) 0.12524(2) 0.01783(15) Uani 1 1 d . . .
P2 P 0.80437(6) 0.29944(7) 0.05755(2) 0.01603(14) Uani 1 1 d . . .
O1 O 0.5895(3) 0.1040(4) 0.00505(9) 0.0586(10) Uani 1 1 d . . .
O2 O 0.8878(2) 0.0551(2) 0.14871(8) 0.0283(5) Uani 1 1 d . . .
N1 N 0.71255(19) 0.2781(2) 0.14141(7) 0.0159(4) Uani 1 1 d . . .
N2 N 0.5573(2) 0.1634(3) 0.17346(8) 0.0193(4) Uani 1 1 d . . .
N3 N 0.8511(2) 0.4016(3) 0.10224(8) 0.0180(4) Uani 1 1 d . . .
C1 C 0.6373(2) 0.2697(3) 0.17607(9) 0.0173(5) Uani 1 1 d . . .
C2 C 0.6415(3) 0.3640(3) 0.21264(10) 0.0233(6) Uani 1 1 d . . .
H2 H 0.5901 0.3548 0.2371 0.028 Uiso 1 1 calc R . .
C3 C 0.7215(3) 0.4700(3) 0.21240(10) 0.0263(6) Uani 1 1 d . . .
H3 H 0.7276 0.5321 0.2376 0.032 Uiso 1 1 calc R . .
C4 C 0.7934(3) 0.4880(3) 0.17598(10) 0.0227(6) Uani 1 1 d . . .
H4 H 0.8465 0.5636 0.1752 0.027 Uiso 1 1 calc R . .
C5 C 0.7849(2) 0.3907(3) 0.14048(9) 0.0167(5) Uani 1 1 d . . .
C6 C 0.5369(3) -0.1163(3) 0.14604(12) 0.0270(6) Uani 1 1 d . . .
H6 H 0.4684 -0.1183 0.1660 0.032 Uiso 1 1 calc R . .
C7 C 0.5109(4) -0.2161(4) 0.10611(15) 0.0454(10) Uani 1 1 d . . .
H7A H 0.5727 -0.2089 0.0841 0.068 Uiso 1 1 calc R . .
H7B H 0.4360 -0.1915 0.0910 0.068 Uiso 1 1 calc R . .
H7C H 0.5074 -0.3115 0.1177 0.068 Uiso 1 1 calc R . .
C8 C 0.6431(4) -0.1625(4) 0.17498(15) 0.0416(9) Uani 1 1 d . . .
H8A H 0.6259 -0.2505 0.1902 0.062 Uiso 1 1 calc R . .
H8B H 0.6624 -0.0914 0.1981 0.062 Uiso 1 1 calc R . .
H8C H 0.7092 -0.1754 0.1553 0.062 Uiso 1 1 calc R . .
C9 C 0.4137(3) 0.0943(5) 0.09374(13) 0.0366(8) Uani 1 1 d . . .
H9 H 0.4153 0.0374 0.0652 0.044 Uiso 1 1 calc R . .
C10 C 0.4026(4) 0.2444(6) 0.0788(2) 0.074(2) Uani 1 1 d . . .
H10A H 0.3272 0.2583 0.0625 0.111 Uiso 1 1 calc R . .
H10B H 0.4655 0.2671 0.0584 0.111 Uiso 1 1 calc R . .
H10C H 0.4079 0.3050 0.1057 0.111 Uiso 1 1 calc R . .
C11 C 0.3037(3) 0.0506(5) 0.11841(15) 0.0433(10) Uani 1 1 d . . .
H11A H 0.2899 0.1162 0.1433 0.065 Uiso 1 1 calc R . .
H11B H 0.3146 -0.0431 0.1310 0.065 Uiso 1 1 calc R . .
H11C H 0.2366 0.0510 0.0966 0.065 Uiso 1 1 calc R . .
C12 C 0.9337(3) 0.2640(3) 0.02501(10) 0.0214(5) Uani 1 1 d . . .
H12 H 0.9635 0.3549 0.0137 0.026 Uiso 1 1 calc R . .
C13 C 0.8976(3) 0.1753(4) -0.01705(11) 0.0297(7) Uani 1 1 d . . .
H13A H 0.9645 0.1636 -0.0364 0.044 Uiso 1 1 calc R . .
H13B H 0.8344 0.2219 -0.0346 0.044 Uiso 1 1 calc R . .
H13C H 0.8709 0.0840 -0.0070 0.044 Uiso 1 1 calc R . .
C14 C 1.0309(3) 0.1960(3) 0.05438(11) 0.0270(6) Uani 1 1 d . . .
H14A H 1.0037 0.1066 0.0660 0.041 Uiso 1 1 calc R . .
H14B H 1.0526 0.2570 0.0802 0.041 Uiso 1 1 calc R . .
H14C H 1.0988 0.1808 0.0358 0.041 Uiso 1 1 calc R . .
C15 C 0.7115(3) 0.4129(3) 0.02047(10) 0.0265(6) Uani 1 1 d . . .
H15 H 0.6612 0.3517 0.0003 0.032 Uiso 1 1 calc R . .
C16 C 0.6311(3) 0.4984(4) 0.05044(12) 0.0297(7) Uani 1 1 d . . .
H16A H 0.6771 0.5683 0.0675 0.045 Uiso 1 1 calc R . .
H16B H 0.5934 0.4364 0.0719 0.045 Uiso 1 1 calc R . .
H16C H 0.5715 0.5448 0.0309 0.045 Uiso 1 1 calc R . .
C17 C 0.7786(4) 0.5109(5) -0.01059(14) 0.0439(10) Uani 1 1 d . . .
H17A H 0.7233 0.5659 -0.0295 0.066 Uiso 1 1 calc R . .
H17B H 0.8277 0.4559 -0.0304 0.066 Uiso 1 1 calc R . .
H17C H 0.8278 0.5734 0.0083 0.066 Uiso 1 1 calc R . .
C18 C 0.4741(3) 0.1495(4) 0.21015(11) 0.0276(6) Uani 1 1 d . . .
H18A H 0.5169 0.1365 0.2395 0.041 Uiso 1 1 calc R . .
H18B H 0.4236 0.0690 0.2039 0.041 Uiso 1 1 calc R . .
H18C H 0.4264 0.2338 0.2114 0.041 Uiso 1 1 calc R . .
C19 C 0.9278(3) 0.5227(3) 0.09775(11) 0.0272(6) Uani 1 1 d . . .
H19A H 0.8807 0.6076 0.0961 0.041 Uiso 1 1 calc R . .
H19B H 0.9713 0.5137 0.0698 0.041 Uiso 1 1 calc R . .
H19C H 0.9824 0.5275 0.1243 0.041 Uiso 1 1 calc R . .
C20 C 0.6426(3) 0.1017(4) 0.03973(11) 0.0348(8) Uani 1 1 d . . .
C21 C 0.9557(4) -0.0736(4) 0.15597(16) 0.0422(9) Uani 1 1 d . . .
H21A H 1.0186 -0.0799 0.1340 0.051 Uiso 1 1 calc R . .
H21B H 0.9051 -0.1565 0.1524 0.051 Uiso 1 1 calc R . .
C22 C 1.0058(4) -0.0625(5) 0.20466(16) 0.0493(11) Uani 1 1 d . . .
H22A H 0.9475 -0.0885 0.2271 0.059 Uiso 1 1 calc R . .
H22B H 1.0756 -0.1221 0.2094 0.059 Uiso 1 1 calc R . .
C23 C 1.0367(3) 0.0885(5) 0.20823(14) 0.0410(9) Uani 1 1 d . . .
H23A H 1.1114 0.1081 0.1938 0.049 Uiso 1 1 calc R . .
H23B H 1.0421 0.1193 0.2405 0.049 Uiso 1 1 calc R . .
C24 C 0.9353(3) 0.1580(4) 0.18220(12) 0.0324(7) Uani 1 1 d . . .
H24A H 0.8748 0.1857 0.2035 0.039 Uiso 1 1 calc R . .
H24B H 0.9622 0.2420 0.1662 0.039 Uiso 1 1 calc R . .
Sb1 Sb 0.24146(10) 0.56080(11) 0.17954(8) 0.03307(19) Uani 1 1 d . . .
F1 F 0.1901(4) 0.3832(4) 0.1686(3) 0.181(4) Uani 1 1 d . . .
F2 F 0.2996(4) 0.7405(4) 0.18612(11) 0.0854(12) Uani 1 1 d . . .
F3 F 0.2200(3) 0.5994(6) 0.11675(10) 0.0997(16) Uani 1 1 d . . .
F4 F 0.2638(4) 0.5412(7) 0.24145(15) 0.148(3) Uani 1 1 d . . .
F5 F 0.0927(3) 0.6123(4) 0.18910(10) 0.0672(9) Uani 1 1 d . . .
F6 F 0.3953(3) 0.5039(5) 0.1692(2) 0.1185(19) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C20 1.913(4) . ?
Mo1 N1 2.260(2) . ?
Mo1 O2 2.312(3) . ?
Mo1 P2 2.3717(8) . ?
Mo1 P1 2.3853(9) . ?
Mo1 Cl1 2.3966(8) . ?
P1 N2 1.705(3) . ?
P1 C9 1.835(3) . ?
P1 C6 1.845(3) . ?
P2 N3 1.704(2) . ?
P2 C12 1.830(3) . ?
P2 C15 1.847(3) . ?
O1 C20 1.162(5) . ?
O2 C21 1.474(4) . ?
O2 C24 1.481(4) . ?
N1 C1 1.362(3) . ?
N1 C5 1.366(4) . ?
N2 C1 1.376(4) . ?
N2 C18 1.473(3) . ?
N3 C5 1.383(3) . ?
N3 C19 1.470(4) . ?
C1 C2 1.401(4) . ?
C2 C3 1.373(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.398(4) . ?
C4 H4 0.9500 . ?
C6 C8 1.522(5) . ?
C6 C7 1.531(5) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.512(6) . ?
C9 C11 1.540(5) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.528(4) . ?
C12 C13 1.540(4) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.538(4) . ?
C15 C17 1.539(5) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 C22 1.518(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.497(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.520(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
Sb1 F5 1.813(3) . ?
Sb1 F4 1.828(4) . ?
Sb1 F1 1.831(4) . ?
Sb1 F2 1.860(3) . ?
Sb1 F3 1.880(4) . ?
Sb1 F6 1.888(4) . ?

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
C20 Mo1 N1 113.20(14) . . ?
C20 Mo1 O2 165.21(13) . . ?
N1 Mo1 O2 80.18(9) . . ?
C20 Mo1 P2 77.13(11) . . ?
N1 Mo1 P2 71.82(6) . . ?
O2 Mo1 P2 102.49(7) . . ?
C20 Mo1 P1 79.42(11) . . ?
N1 Mo1 P1 73.80(6) . . ?
O2 Mo1 P1 111.56(7) . . ?
P2 Mo1 P1 125.66(4) . . ?
C20 Mo1 Cl1 83.79(13) . . ?
N1 Mo1 Cl1 162.97(9) . . ?
O2 Mo1 Cl1 83.09(7) . . ?
P2 Mo1 Cl1 115.27(3) . . ?
P1 Mo1 Cl1 109.91(3) . . ?
N2 P1 C9 108.67(17) . . ?
N2 P1 C6 104.79(14) . . ?
C9 P1 C6 102.79(17) . . ?
N2 P1 Mo1 104.05(9) . . ?
C9 P1 Mo1 124.66(12) . . ?
C6 P1 Mo1 110.41(10) . . ?
N3 P2 C12 105.63(13) . . ?
N3 P2 C15 105.42(13) . . ?
C12 P2 C15 105.47(14) . . ?
N3 P2 Mo1 102.87(9) . . ?
C12 P2 Mo1 111.04(10) . . ?
C15 P2 Mo1 124.83(12) . . ?
C21 O2 C24 106.7(3) . . ?
C21 O2 Mo1 127.7(2) . . ?
C24 O2 Mo1 125.64(18) . . ?
C1 N1 C5 117.9(2) . . ?
C1 N1 Mo1 120.99(18) . . ?
C5 N1 Mo1 120.26(17) . . ?
C1 N2 C18 118.7(2) . . ?
C1 N2 P1 117.53(18) . . ?
C18 N2 P1 123.6(2) . . ?
C5 N3 C19 119.0(2) . . ?
C5 N3 P2 114.23(19) . . ?
C19 N3 P2 124.02(19) . . ?
N1 C1 N2 116.5(2) . . ?
N1 C1 C2 121.8(3) . . ?
N2 C1 C2 121.7(2) . . ?
C3 C2 C1 118.6(3) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C2 C3 C4 121.2(3) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C3 C4 C5 117.5(3) . . ?
C3 C4 H4 121.2 . . ?
C5 C4 H4 121.2 . . ?
N1 C5 N3 115.6(2) . . ?
N1 C5 C4 122.6(3) . . ?
N3 C5 C4 121.8(3) . . ?
C8 C6 C7 111.6(3) . . ?
C8 C6 P1 111.7(2) . . ?
C7 C6 P1 110.8(3) . . ?
C8 C6 H6 107.5 . . ?
C7 C6 H6 107.5 . . ?
P1 C6 H6 107.5 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C11 109.6(4) . . ?
C10 C9 P1 111.2(3) . . ?
C11 C9 P1 115.8(3) . . ?
C10 C9 H9 106.6 . . ?
C11 C9 H9 106.6 . . ?
P1 C9 H9 106.6 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C14 C12 C13 112.2(3) . . ?
C14 C12 P2 112.2(2) . . ?
C13 C12 P2 108.7(2) . . ?
C14 C12 H12 107.8 . . ?
C13 C12 H12 107.8 . . ?
P2 C12 H12 107.8 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C17 109.7(3) . . ?
C16 C15 P2 109.1(2) . . ?
C17 C15 P2 114.6(2) . . ?
C16 C15 H15 107.7 . . ?
C17 C15 H15 107.7 . . ?
P2 C15 H15 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O1 C20 Mo1 175.9(3) . . ?
O2 C21 C22 104.8(3) . . ?
O2 C21 H21A 110.8 . . ?
C22 C21 H21A 110.8 . . ?
O2 C21 H21B 110.8 . . ?
C22 C21 H21B 110.8 . . ?
H21A C21 H21B 108.9 . . ?
C23 C22 C21 102.3(3) . . ?
C23 C22 H22A 111.3 . . ?
C21 C22 H22A 111.3 . . ?
C23 C22 H22B 111.3 . . ?
C21 C22 H22B 111.3 . . ?
H22A C22 H22B 109.2 . . ?
C22 C23 C24 102.5(3) . . ?
C22 C23 H23A 111.3 . . ?
C24 C23 H23A 111.3 . . ?
C22 C23 H23B 111.3 . . ?
C24 C23 H23B 111.3 . . ?
H23A C23 H23B 109.2 . . ?
O2 C24 C23 107.0(3) . . ?
O2 C24 H24A 110.3 . . ?
C23 C24 H24A 110.3 . . ?
O2 C24 H24B 110.3 . . ?
C23 C24 H24B 110.3 . . ?
H24A C24 H24B 108.6 . . ?
F5 Sb1 F4 88.3(2) . . ?
F5 Sb1 F1 88.99(19) . . ?
F4 Sb1 F1 96.2(4) . . ?
F5 Sb1 F2 93.87(19) . . ?
F4 Sb1 F2 87.6(2) . . ?
F1 Sb1 F2 175.3(3) . . ?
F5 Sb1 F3 90.61(16) . . ?
F4 Sb1 F3 174.5(3) . . ?
F1 Sb1 F3 89.2(3) . . ?
F2 Sb1 F3 87.1(2) . . ?
F5 Sb1 F6 178.9(2) . . ?
F4 Sb1 F6 92.0(3) . . ?
F1 Sb1 F6 89.9(2) . . ?
F2 Sb1 F6 87.2(2) . . ?
F3 Sb1 F6 89.2(2) . . ?

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
C20 Mo1 P1 N2 -138.59(15) . . . . ?
N1 Mo1 P1 N2 -20.46(11) . . . . ?
O2 Mo1 P1 N2 51.74(11) . . . . ?
P2 Mo1 P1 N2 -72.99(11) . . . . ?
Cl1 Mo1 P1 N2 142.05(10) . . . . ?
C20 Mo1 P1 C9 -13.5(2) . . . . ?
N1 Mo1 P1 C9 104.59(19) . . . . ?
O2 Mo1 P1 C9 176.78(19) . . . . ?
P2 Mo1 P1 C9 52.06(19) . . . . ?
Cl1 Mo1 P1 C9 -92.90(18) . . . . ?
C20 Mo1 P1 C6 109.45(17) . . . . ?
N1 Mo1 P1 C6 -132.42(14) . . . . ?
O2 Mo1 P1 C6 -60.23(14) . . . . ?
P2 Mo1 P1 C6 175.05(13) . . . . ?
Cl1 Mo1 P1 C6 30.09(14) . . . . ?
C20 Mo1 P2 N3 150.54(15) . . . . ?
N1 Mo1 P2 N3 30.52(11) . . . . ?
O2 Mo1 P2 N3 -44.62(10) . . . . ?
P1 Mo1 P2 N3 83.85(11) . . . . ?
Cl1 Mo1 P2 N3 -132.80(10) . . . . ?
C20 Mo1 P2 C12 -96.88(16) . . . . ?
N1 Mo1 P2 C12 143.10(12) . . . . ?
O2 Mo1 P2 C12 67.96(12) . . . . ?
P1 Mo1 P2 C12 -163.57(11) . . . . ?
Cl1 Mo1 P2 C12 -20.22(13) . . . . ?
C20 Mo1 P2 C15 31.12(17) . . . . ?
N1 Mo1 P2 C15 -88.90(14) . . . . ?
O2 Mo1 P2 C15 -164.03(14) . . . . ?
P1 Mo1 P2 C15 -35.56(14) . . . . ?
Cl1 Mo1 P2 C15 107.79(14) . . . . ?
C20 Mo1 O2 C21 -39.1(6) . . . . ?
N1 Mo1 O2 C21 165.4(3) . . . . ?
P2 Mo1 O2 C21 -125.9(3) . . . . ?
P1 Mo1 O2 C21 97.2(3) . . . . ?
Cl1 Mo1 O2 C21 -11.5(3) . . . . ?
C20 Mo1 O2 C24 138.5(5) . . . . ?
N1 Mo1 O2 C24 -17.0(2) . . . . ?
P2 Mo1 O2 C24 51.7(2) . . . . ?
P1 Mo1 O2 C24 -85.1(2) . . . . ?
Cl1 Mo1 O2 C24 166.1(2) . . . . ?
C20 Mo1 N1 C1 94.0(2) . . . . ?
O2 Mo1 N1 C1 -92.6(2) . . . . ?
P2 Mo1 N1 C1 160.7(2) . . . . ?
P1 Mo1 N1 C1 23.42(19) . . . . ?
Cl1 Mo1 N1 C1 -81.8(3) . . . . ?
C20 Mo1 N1 C5 -96.9(2) . . . . ?
O2 Mo1 N1 C5 76.5(2) . . . . ?
P2 Mo1 N1 C5 -30.18(18) . . . . ?
P1 Mo1 N1 C5 -167.4(2) . . . . ?
Cl1 Mo1 N1 C5 87.4(3) . . . . ?
C9 P1 N2 C1 -112.8(2) . . . . ?
C6 P1 N2 C1 137.8(2) . . . . ?
Mo1 P1 N2 C1 21.9(2) . . . . ?
C9 P1 N2 C18 61.7(3) . . . . ?
C6 P1 N2 C18 -47.7(3) . . . . ?
Mo1 P1 N2 C18 -163.6(2) . . . . ?
C12 P2 N3 C5 -153.0(2) . . . . ?
C15 P2 N3 C5 95.6(2) . . . . ?
Mo1 P2 N3 C5 -36.5(2) . . . . ?
C12 P2 N3 C19 46.2(3) . . . . ?
C15 P2 N3 C19 -65.2(3) . . . . ?
Mo1 P2 N3 C19 162.7(2) . . . . ?
C5 N1 C1 N2 173.3(2) . . . . ?
Mo1 N1 C1 N2 -17.3(3) . . . . ?
C5 N1 C1 C2 -7.0(4) . . . . ?
Mo1 N1 C1 C2 162.4(2) . . . . ?
C18 N2 C1 N1 179.9(3) . . . . ?
P1 N2 C1 N1 -5.4(3) . . . . ?
C18 N2 C1 C2 0.1(4) . . . . ?
P1 N2 C1 C2 174.9(2) . . . . ?
N1 C1 C2 C3 2.1(4) . . . . ?
N2 C1 C2 C3 -178.2(3) . . . . ?
C1 C2 C3 C4 2.9(5) . . . . ?
C2 C3 C4 C5 -2.7(5) . . . . ?
C1 N1 C5 N3 -173.7(2) . . . . ?
Mo1 N1 C5 N3 16.8(3) . . . . ?
C1 N1 C5 C4 7.2(4) . . . . ?
Mo1 N1 C5 C4 -162.3(2) . . . . ?
C19 N3 C5 N1 177.6(3) . . . . ?
P2 N3 C5 N1 15.7(3) . . . . ?
C19 N3 C5 C4 -3.3(4) . . . . ?
P2 N3 C5 C4 -165.2(2) . . . . ?
C3 C4 C5 N1 -2.4(4) . . . . ?
C3 C4 C5 N3 178.5(3) . . . . ?
N2 P1 C6 C8 -64.6(3) . . . . ?
C9 P1 C6 C8 -178.1(3) . . . . ?
Mo1 P1 C6 C8 46.9(3) . . . . ?
N2 P1 C6 C7 170.4(2) . . . . ?
C9 P1 C6 C7 56.9(3) . . . . ?
Mo1 P1 C6 C7 -78.1(3) . . . . ?
N2 P1 C9 C10 62.0(4) . . . . ?
C6 P1 C9 C10 172.7(4) . . . . ?
Mo1 P1 C9 C10 -61.0(4) . . . . ?
N2 P1 C9 C11 -63.9(4) . . . . ?
C6 P1 C9 C11 46.8(4) . . . . ?
Mo1 P1 C9 C11 173.1(3) . . . . ?
N3 P2 C12 C14 56.9(2) . . . . ?
C15 P2 C12 C14 168.3(2) . . . . ?
Mo1 P2 C12 C14 -53.9(2) . . . . ?
N3 P2 C12 C13 -178.3(2) . . . . ?
C15 P2 C12 C13 -67.0(2) . . . . ?
Mo1 P2 C12 C13 70.9(2) . . . . ?
N3 P2 C15 C16 -44.1(3) . . . . ?
C12 P2 C15 C16 -155.6(2) . . . . ?
Mo1 P2 C15 C16 74.2(3) . . . . ?
N3 P2 C15 C17 79.4(3) . . . . ?
C12 P2 C15 C17 -32.1(3) . . . . ?
Mo1 P2 C15 C17 -162.3(2) . . . . ?
C24 O2 C21 C22 22.5(4) . . . . ?
Mo1 O2 C21 C22 -159.5(2) . . . . ?
O2 C21 C22 C23 -38.9(4) . . . . ?
C21 C22 C23 C24 39.2(4) . . . . ?
C21 O2 C24 C23 2.3(4) . . . . ?
Mo1 O2 C24 C23 -175.8(2) . . . . ?
C22 C23 C24 O2 -26.3(4) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.476
_refine_diff_density_min         -1.524
_refine_diff_density_rms         0.112
_database_code_depnum_ccdc_archive 'CCDC 1004522'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4b-1702

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
4b-1702 [Mo(PNPMe-iPr)(CO)Br2], crystal form 2 of 2, polymorph of
4-1680 [Mo(PNPMe-iPr)(CO)Br2], 
Dibromo-carbonyl-[N,N'-bis(diisopropylphosphino)-N,N'-dimethyl-2,6-
diaminopyridine-\kP,N¹,P']-molybdenum(iv)
;
_chemical_name_common            
'4b-1702 [Mo(PNPMe-iPr)(CO)Br2], crystal form 2'
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H37 Br2 Mo N3 O P2'
_chemical_formula_sum            'C20 H37 Br2 Mo N3 O P2'
_chemical_formula_weight         653.23

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '

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

_cell_length_a                   19.1328(5)
_cell_length_b                   8.9912(2)
_cell_length_c                   29.1561(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.475(2)
_cell_angle_gamma                90.00
_cell_volume                     5011.0(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9899
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      30.07

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2624
_exptl_absorpt_coefficient_mu    3.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
; 
4b-1702 [Mo(PNPMe-iPr)(CO)Br2] is the second polymorph
of the complex [Mo(PNPMe-iPr)(CO)Br2] which has a 
higher density of 1.732 g/cm3 than the first polymorph
which is reported as 4-1680 [Mo(PNPMe-iPr)(CO)Br2]
in this CIF and which has a density 1.666 g/cm3.
It seems that 4-1680 is a kinetically favoured 
crystal form whereas 4b-1702 should be a thermodynamically
favoured form. The [Mo(PNPMe-iPr)(CO)Br2] complexes
in both polymorphs are very similar in bond lengths,
bond angles and general conformation but differ in the 
orientation of one out of four isopropyl groups (C9,C10,C11). 
This isopropyl group has a torsion angle of 
Mo1-P1-C9-H9 = 42.3 deg in 4-1680 and 166.6 deg in 4b-1702,
(first complex in 4b-1702, the independent second complex in 4b-1702 
is very similar).
Due to ineficient packing the structure of 4-1680 contains 
solvent accessible voids of ca. 50 A³ (unoccupied, no solvent
electron density detected), whereas the structure of 4b-1702
has no solvent accessible voids.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            127063
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         1.72
_diffrn_reflns_theta_max         30.00
_reflns_number_total             14602
_reflns_number_gt                12024
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0164P)²+9.7330P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14602
_refine_ls_number_parameters     543
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.0663
_refine_ls_wR_factor_gt          0.0625
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_restrained_S_all      1.160
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.114720(11) 0.58875(2) 0.376251(7) 0.00877(4) Uani 1 1 d . . .
Mo2 Mo 0.384517(11) 0.46037(2) 0.121036(7) 0.00926(4) Uani 1 1 d . . .
Br1 Br 0.048672(14) 0.81490(3) 0.405529(9) 0.01600(6) Uani 1 1 d . . .
Br2 Br 0.087191(14) 0.70310(3) 0.294500(9) 0.01694(6) Uani 1 1 d . . .
Br3 Br 0.452190(14) 0.23368(3) 0.094004(9) 0.01633(6) Uani 1 1 d . . .
Br4 Br 0.409320(15) 0.34968(3) 0.203546(9) 0.01848(6) Uani 1 1 d . . .
P1 P 0.04618(3) 0.36882(7) 0.37931(2) 0.01044(12) Uani 1 1 d . . .
P2 P 0.23779(3) 0.61546(7) 0.38680(2) 0.01133(12) Uani 1 1 d . . .
P3 P 0.26220(3) 0.43311(7) 0.10616(2) 0.01153(12) Uani 1 1 d . . .
P4 P 0.45246(3) 0.68129(7) 0.12021(2) 0.01138(12) Uani 1 1 d . . .
N1 N 0.16775(11) 0.4176(2) 0.33120(7) 0.0116(4) Uani 1 1 d . . .
N2 N 0.06969(11) 0.2649(2) 0.33340(7) 0.0138(4) Uani 1 1 d . . .
N3 N 0.26844(11) 0.5631(3) 0.33501(7) 0.0140(4) Uani 1 1 d . . .
N4 N 0.32730(11) 0.6310(2) 0.16426(7) 0.0120(4) Uani 1 1 d . . .
N5 N 0.22793(11) 0.4815(3) 0.15715(7) 0.0147(4) Uani 1 1 d . . .
N6 N 0.42440(12) 0.7868(2) 0.16447(7) 0.0151(4) Uani 1 1 d . . .
O1 O 0.13595(10) 0.5372(2) 0.48047(6) 0.0175(4) Uani 1 1 d . . .
O2 O 0.37230(10) 0.5085(2) 0.01617(6) 0.0192(4) Uani 1 1 d . . .
C1 C 0.13311(14) 0.2945(3) 0.31500(8) 0.0132(5) Uani 1 1 d . . .
C2 C 0.16059(15) 0.2006(3) 0.28201(9) 0.0175(5) Uani 1 1 d . . .
H2 H 0.1353 0.1159 0.2711 0.021 Uiso 1 1 calc R . .
C3 C 0.22523(16) 0.2339(3) 0.26566(9) 0.0203(6) Uani 1 1 d . . .
H3 H 0.2446 0.1718 0.2431 0.024 Uiso 1 1 calc R . .
C4 C 0.26208(15) 0.3562(3) 0.28164(9) 0.0191(5) Uani 1 1 d . . .
H4 H 0.3065 0.3799 0.2703 0.023 Uiso 1 1 calc R . .
C5 C 0.23220(13) 0.4443(3) 0.31495(9) 0.0137(5) Uani 1 1 d . . .
C6 C -0.04848(13) 0.4029(3) 0.36783(9) 0.0163(5) Uani 1 1 d . . .
H6 H -0.0730 0.3065 0.3731 0.020 Uiso 1 1 calc R . .
C7 C -0.07820(14) 0.5165(3) 0.40119(11) 0.0228(6) Uani 1 1 d . . .
H7A H -0.0663 0.6173 0.3914 0.034 Uiso 1 1 calc R . .
H7B H -0.0581 0.4985 0.4322 0.034 Uiso 1 1 calc R . .
H7C H -0.1292 0.5060 0.4013 0.034 Uiso 1 1 calc R . .
C8 C -0.06697(15) 0.4491(4) 0.31835(10) 0.0255(6) Uani 1 1 d . . .
H8A H -0.1179 0.4583 0.3140 0.038 Uiso 1 1 calc R . .
H8B H -0.0499 0.3736 0.2973 0.038 Uiso 1 1 calc R . .
H8C H -0.0450 0.5449 0.3120 0.038 Uiso 1 1 calc R . .
C9 C 0.04675(13) 0.2277(3) 0.42542(9) 0.0135(5) Uani 1 1 d . . .
H9 H 0.0208 0.1397 0.4124 0.016 Uiso 1 1 calc R . .
C10 C 0.01007(15) 0.2711(3) 0.46906(9) 0.0206(6) Uani 1 1 d . . .
H10A H 0.0166 0.1921 0.4920 0.031 Uiso 1 1 calc R . .
H10B H -0.0400 0.2851 0.4618 0.031 Uiso 1 1 calc R . .
H10C H 0.0302 0.3640 0.4813 0.031 Uiso 1 1 calc R . .
C11 C 0.12165(14) 0.1753(3) 0.43629(10) 0.0178(5) Uani 1 1 d . . .
H11A H 0.1473 0.2526 0.4537 0.027 Uiso 1 1 calc R . .
H11B H 0.1449 0.1559 0.4076 0.027 Uiso 1 1 calc R . .
H11C H 0.1208 0.0839 0.4546 0.027 Uiso 1 1 calc R . .
C12 C 0.26418(14) 0.8107(3) 0.39460(9) 0.0155(5) Uani 1 1 d . . .
H12 H 0.3163 0.8149 0.3933 0.019 Uiso 1 1 calc R . .
C13 C 0.24516(15) 0.8631(3) 0.44240(9) 0.0197(6) Uani 1 1 d . . .
H13A H 0.2608 0.9659 0.4470 0.030 Uiso 1 1 calc R . .
H13B H 0.2681 0.7990 0.4657 0.030 Uiso 1 1 calc R . .
H13C H 0.1943 0.8577 0.4451 0.030 Uiso 1 1 calc R . .
C14 C 0.23369(15) 0.9123(3) 0.35704(9) 0.0191(5) Uani 1 1 d . . .
H14A H 0.1826 0.9136 0.3582 0.029 Uiso 1 1 calc R . .
H14B H 0.2470 0.8754 0.3270 0.029 Uiso 1 1 calc R . .
H14C H 0.2519 1.0133 0.3617 0.029 Uiso 1 1 calc R . .
C15 C 0.29253(14) 0.5138(3) 0.43023(9) 0.0167(5) Uani 1 1 d . . .
H15 H 0.2702 0.5253 0.4604 0.020 Uiso 1 1 calc R . .
C16 C 0.29207(15) 0.3473(3) 0.41839(10) 0.0205(6) Uani 1 1 d . . .
H16A H 0.3174 0.3313 0.3903 0.031 Uiso 1 1 calc R . .
H16B H 0.2437 0.3132 0.4136 0.031 Uiso 1 1 calc R . .
H16C H 0.3149 0.2913 0.4437 0.031 Uiso 1 1 calc R . .
C17 C 0.36815(14) 0.5701(3) 0.43624(10) 0.0223(6) Uani 1 1 d . . .
H17A H 0.3937 0.5093 0.4593 0.033 Uiso 1 1 calc R . .
H17B H 0.3680 0.6740 0.4464 0.033 Uiso 1 1 calc R . .
H17C H 0.3911 0.5629 0.4069 0.033 Uiso 1 1 calc R . .
C18 C 0.03097(15) 0.1307(3) 0.31798(10) 0.0191(6) Uani 1 1 d . . .
H18A H 0.0199 0.1375 0.2849 0.029 Uiso 1 1 calc R . .
H18B H -0.0125 0.1232 0.3344 0.029 Uiso 1 1 calc R . .
H18C H 0.0598 0.0424 0.3244 0.029 Uiso 1 1 calc R . .
C19 C 0.33858(14) 0.5959(3) 0.31916(10) 0.0205(6) Uani 1 1 d . . .
H19A H 0.3693 0.5105 0.3254 0.031 Uiso 1 1 calc R . .
H19B H 0.3575 0.6835 0.3354 0.031 Uiso 1 1 calc R . .
H19C H 0.3357 0.6157 0.2861 0.031 Uiso 1 1 calc R . .
C20 C 0.12760(13) 0.5508(3) 0.44097(9) 0.0131(5) Uani 1 1 d . . .
C21 C 0.26173(13) 0.6016(3) 0.17833(9) 0.0141(5) Uani 1 1 d . . .
C22 C 0.22891(15) 0.6887(3) 0.21053(9) 0.0198(6) Uani 1 1 d . . .
H22 H 0.1840 0.6631 0.2208 0.024 Uiso 1 1 calc R . .
C23 C 0.26378(16) 0.8137(3) 0.22719(9) 0.0219(6) Uani 1 1 d . . .
H23 H 0.2423 0.8757 0.2489 0.026 Uiso 1 1 calc R . .
C24 C 0.32909(16) 0.8494(3) 0.21273(9) 0.0201(6) Uani 1 1 d . . .
H24 H 0.3528 0.9357 0.2240 0.024 Uiso 1 1 calc R . .
C25 C 0.36008(14) 0.7557(3) 0.18090(8) 0.0141(5) Uani 1 1 d . . .
C26 C 0.23670(14) 0.2386(3) 0.09636(9) 0.0158(5) Uani 1 1 d . . .
H26 H 0.1845 0.2340 0.0962 0.019 Uiso 1 1 calc R . .
C27 C 0.25879(15) 0.1884(3) 0.04901(10) 0.0203(6) Uani 1 1 d . . .
H27A H 0.3099 0.1924 0.0479 0.031 Uiso 1 1 calc R . .
H27B H 0.2379 0.2545 0.0255 0.031 Uiso 1 1 calc R . .
H27C H 0.2428 0.0863 0.0433 0.031 Uiso 1 1 calc R . .
C28 C 0.26497(15) 0.1353(3) 0.13466(10) 0.0195(6) Uani 1 1 d . . .
H28A H 0.2485 0.0336 0.1286 0.029 Uiso 1 1 calc R . .
H28B H 0.2482 0.1691 0.1642 0.029 Uiso 1 1 calc R . .
H28C H 0.3162 0.1370 0.1357 0.029 Uiso 1 1 calc R . .
C29 C 0.21049(13) 0.5380(3) 0.06194(9) 0.0152(5) Uani 1 1 d . . .
H29 H 0.2349 0.5273 0.0325 0.018 Uiso 1 1 calc R . .
C30 C 0.21078(15) 0.7037(3) 0.07404(10) 0.0207(6) Uani 1 1 d . . .
H30A H 0.1898 0.7605 0.0483 0.031 Uiso 1 1 calc R . .
H30B H 0.2591 0.7370 0.0802 0.031 Uiso 1 1 calc R . .
H30C H 0.1837 0.7197 0.1014 0.031 Uiso 1 1 calc R . .
C31 C 0.13514(15) 0.4847(3) 0.05298(10) 0.0231(6) Uani 1 1 d . . .
H31A H 0.1095 0.4936 0.0812 0.035 Uiso 1 1 calc R . .
H31B H 0.1354 0.3805 0.0431 0.035 Uiso 1 1 calc R . .
H31C H 0.1124 0.5459 0.0289 0.035 Uiso 1 1 calc R . .
C32 C 0.54643(14) 0.6494(3) 0.13531(10) 0.0187(5) Uani 1 1 d . . .
H32 H 0.5713 0.7449 0.1294 0.022 Uiso 1 1 calc R . .
C33 C 0.57868(15) 0.5303(3) 0.10459(12) 0.0258(7) Uani 1 1 d . . .
H33A H 0.6297 0.5400 0.1062 0.039 Uiso 1 1 calc R . .
H33B H 0.5612 0.5440 0.0728 0.039 Uiso 1 1 calc R . .
H33C H 0.5656 0.4312 0.1153 0.039 Uiso 1 1 calc R . .
C34 C 0.56131(17) 0.6113(4) 0.18585(11) 0.0295(7) Uani 1 1 d . . .
H34A H 0.5388 0.5166 0.1929 0.044 Uiso 1 1 calc R . .
H34B H 0.5427 0.6900 0.2051 0.044 Uiso 1 1 calc R . .
H34C H 0.6119 0.6027 0.1919 0.044 Uiso 1 1 calc R . .
C35 C 0.45631(14) 0.8201(3) 0.07348(9) 0.0157(5) Uani 1 1 d . . .
H35 H 0.4816 0.9083 0.0868 0.019 Uiso 1 1 calc R . .
C36 C 0.49661(15) 0.7715(3) 0.03182(10) 0.0199(6) Uani 1 1 d . . .
H36A H 0.4762 0.6796 0.0191 0.030 Uiso 1 1 calc R . .
H36B H 0.5457 0.7541 0.0412 0.030 Uiso 1 1 calc R . .
H36C H 0.4938 0.8497 0.0084 0.030 Uiso 1 1 calc R . .
C37 C 0.38284(14) 0.8731(3) 0.05935(10) 0.0186(5) Uani 1 1 d . . .
H37A H 0.3859 0.9630 0.0405 0.028 Uiso 1 1 calc R . .
H37B H 0.3571 0.8955 0.0869 0.028 Uiso 1 1 calc R . .
H37C H 0.3583 0.7950 0.0416 0.028 Uiso 1 1 calc R . .
C38 C 0.15684(14) 0.4466(3) 0.17052(10) 0.0220(6) Uani 1 1 d . . .
H38A H 0.1572 0.4267 0.2036 0.033 Uiso 1 1 calc R . .
H38B H 0.1398 0.3586 0.1537 0.033 Uiso 1 1 calc R . .
H38C H 0.1260 0.5311 0.1632 0.033 Uiso 1 1 calc R . .
C39 C 0.46148(16) 0.9215(3) 0.18100(10) 0.0211(6) Uani 1 1 d . . .
H39A H 0.4328 1.0093 0.1737 0.032 Uiso 1 1 calc R . .
H39B H 0.5062 0.9297 0.1660 0.032 Uiso 1 1 calc R . .
H39C H 0.4702 0.9149 0.2143 0.032 Uiso 1 1 calc R . .
C40 C 0.37675(13) 0.4967(3) 0.05610(9) 0.0142(5) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C20 1.923(3) . ?
Mo1 N1 2.289(2) . ?
Mo1 P2 2.3736(7) . ?
Mo1 P1 2.3766(7) . ?
Mo1 Br1 2.5599(3) . ?
Mo1 Br2 2.6282(3) . ?
Mo2 C40 1.921(3) . ?
Mo2 N4 2.293(2) . ?
Mo2 P3 2.3744(7) . ?
Mo2 P4 2.3746(7) . ?
Mo2 Br3 2.5573(3) . ?
Mo2 Br4 2.6276(3) . ?
P1 N2 1.708(2) . ?
P1 C9 1.848(3) . ?
P1 C6 1.853(3) . ?
P2 N3 1.709(2) . ?
P2 C12 1.838(3) . ?
P2 C15 1.850(3) . ?
P3 N5 1.707(2) . ?
P3 C26 1.835(3) . ?
P3 C29 1.849(3) . ?
P4 N6 1.707(2) . ?
P4 C35 1.851(3) . ?
P4 C32 1.855(3) . ?
N1 C5 1.361(3) . ?
N1 C1 1.364(3) . ?
N2 C1 1.374(3) . ?
N2 C18 1.476(3) . ?
N3 C5 1.389(3) . ?
N3 C19 1.468(3) . ?
N4 C21 1.363(3) . ?
N4 C25 1.364(3) . ?
N5 C21 1.389(3) . ?
N5 C38 1.465(3) . ?
N6 C25 1.369(3) . ?
N6 C39 1.474(3) . ?
O1 C20 1.162(3) . ?
O2 C40 1.169(3) . ?
C1 C2 1.399(3) . ?
C2 C3 1.377(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.377(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.395(4) . ?
C4 H4 0.9500 . ?
C6 C8 1.528(4) . ?
C6 C7 1.536(4) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C11 1.529(4) . ?
C9 C10 1.530(4) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.523(4) . ?
C12 C13 1.530(4) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.536(4) . ?
C15 C16 1.536(4) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 C22 1.393(4) . ?
C22 C23 1.385(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.374(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.403(4) . ?
C24 H24 0.9500 . ?
C26 C27 1.529(4) . ?
C26 C28 1.533(4) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C31 1.531(4) . ?
C29 C30 1.531(4) . ?
C29 H29 1.0000 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C34 1.528(4) . ?
C32 C33 1.542(4) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C37 1.524(4) . ?
C35 C36 1.530(4) . ?
C35 H35 1.0000 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?

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
C20 Mo1 N1 113.75(9) . . ?
C20 Mo1 P2 78.84(8) . . ?
N1 Mo1 P2 71.37(6) . . ?
C20 Mo1 P1 82.13(8) . . ?
N1 Mo1 P1 73.80(6) . . ?
P2 Mo1 P1 128.70(2) . . ?
C20 Mo1 Br1 81.83(8) . . ?
N1 Mo1 Br1 164.35(5) . . ?
P2 Mo1 Br1 112.188(19) . . ?
P1 Mo1 Br1 111.547(18) . . ?
C20 Mo1 Br2 166.29(8) . . ?
N1 Mo1 Br2 79.57(5) . . ?
P2 Mo1 Br2 103.695(18) . . ?
P1 Mo1 Br2 105.680(18) . . ?
Br1 Mo1 Br2 84.791(11) . . ?
C40 Mo2 N4 114.16(9) . . ?
C40 Mo2 P3 78.68(8) . . ?
N4 Mo2 P3 71.30(6) . . ?
C40 Mo2 P4 82.34(8) . . ?
N4 Mo2 P4 73.77(6) . . ?
P3 Mo2 P4 128.33(2) . . ?
C40 Mo2 Br3 81.41(8) . . ?
N4 Mo2 Br3 164.27(5) . . ?
P3 Mo2 Br3 111.690(19) . . ?
P4 Mo2 Br3 112.265(19) . . ?
C40 Mo2 Br4 165.97(8) . . ?
N4 Mo2 Br4 79.74(5) . . ?
P3 Mo2 Br4 105.412(19) . . ?
P4 Mo2 Br4 104.410(19) . . ?
Br3 Mo2 Br4 84.633(11) . . ?
N2 P1 C9 101.60(11) . . ?
N2 P1 C6 103.73(12) . . ?
C9 P1 C6 102.71(12) . . ?
N2 P1 Mo1 105.14(8) . . ?
C9 P1 Mo1 127.78(9) . . ?
C6 P1 Mo1 113.09(9) . . ?
N3 P2 C12 105.62(12) . . ?
N3 P2 C15 105.24(12) . . ?
C12 P2 C15 104.05(12) . . ?
N3 P2 Mo1 103.54(8) . . ?
C12 P2 Mo1 112.24(9) . . ?
C15 P2 Mo1 124.60(9) . . ?
N5 P3 C26 105.61(12) . . ?
N5 P3 C29 105.26(12) . . ?
C26 P3 C29 104.30(12) . . ?
N5 P3 Mo2 103.13(8) . . ?
C26 P3 Mo2 112.34(9) . . ?
C29 P3 Mo2 124.62(9) . . ?
N6 P4 C35 101.86(12) . . ?
N6 P4 C32 103.87(12) . . ?
C35 P4 C32 102.11(13) . . ?
N6 P4 Mo2 105.50(8) . . ?
C35 P4 Mo2 127.63(9) . . ?
C32 P4 Mo2 113.19(9) . . ?
C5 N1 C1 117.2(2) . . ?
C5 N1 Mo1 120.78(17) . . ?
C1 N1 Mo1 121.58(17) . . ?
C1 N2 C18 118.6(2) . . ?
C1 N2 P1 117.86(17) . . ?
C18 N2 P1 122.69(18) . . ?
C5 N3 C19 117.9(2) . . ?
C5 N3 P2 113.55(17) . . ?
C19 N3 P2 125.17(18) . . ?
C21 N4 C25 117.9(2) . . ?
C21 N4 Mo2 120.19(17) . . ?
C25 N4 Mo2 121.50(17) . . ?
C21 N5 C38 117.9(2) . . ?
C21 N5 P3 113.35(17) . . ?
C38 N5 P3 124.96(19) . . ?
C25 N6 C39 118.7(2) . . ?
C25 N6 P4 117.90(18) . . ?
C39 N6 P4 122.77(19) . . ?
N1 C1 N2 116.5(2) . . ?
N1 C1 C2 122.4(2) . . ?
N2 C1 C2 121.1(2) . . ?
C3 C2 C1 118.5(3) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C4 C3 C2 120.7(2) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 118.0(3) . . ?
C3 C4 H4 121.0 . . ?
C5 C4 H4 121.0 . . ?
N1 C5 N3 115.6(2) . . ?
N1 C5 C4 123.2(2) . . ?
N3 C5 C4 121.2(2) . . ?
C8 C6 C7 109.9(2) . . ?
C8 C6 P1 113.59(19) . . ?
C7 C6 P1 112.41(19) . . ?
C8 C6 H6 106.8 . . ?
C7 C6 H6 106.8 . . ?
P1 C6 H6 106.8 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C11 C9 C10 111.4(2) . . ?
C11 C9 P1 109.78(18) . . ?
C10 C9 P1 116.18(19) . . ?
C11 C9 H9 106.3 . . ?
C10 C9 H9 106.3 . . ?
P1 C9 H9 106.3 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C14 C12 C13 111.8(2) . . ?
C14 C12 P2 112.91(18) . . ?
C13 C12 P2 109.39(19) . . ?
C14 C12 H12 107.5 . . ?
C13 C12 H12 107.5 . . ?
P2 C12 H12 107.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C17 C15 C16 110.1(2) . . ?
C17 C15 P2 114.70(19) . . ?
C16 C15 P2 109.28(19) . . ?
C17 C15 H15 107.5 . . ?
C16 C15 H15 107.5 . . ?
P2 C15 H15 107.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O1 C20 Mo1 175.8(2) . . ?
N4 C21 N5 115.7(2) . . ?
N4 C21 C22 122.8(3) . . ?
N5 C21 C22 121.5(2) . . ?
C23 C22 C21 118.0(3) . . ?
C23 C22 H22 121.0 . . ?
C21 C22 H22 121.0 . . ?
C24 C23 C22 120.8(3) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 C25 118.6(3) . . ?
C23 C24 H24 120.7 . . ?
C25 C24 H24 120.7 . . ?
N4 C25 N6 116.8(2) . . ?
N4 C25 C24 121.9(3) . . ?
N6 C25 C24 121.4(2) . . ?
C27 C26 C28 112.1(2) . . ?
C27 C26 P3 109.85(19) . . ?
C28 C26 P3 112.40(18) . . ?
C27 C26 H26 107.4 . . ?
C28 C26 H26 107.4 . . ?
P3 C26 H26 107.4 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C31 C29 C30 109.8(2) . . ?
C31 C29 P3 115.52(19) . . ?
C30 C29 P3 109.82(18) . . ?
C31 C29 H29 107.1 . . ?
C30 C29 H29 107.1 . . ?
P3 C29 H29 107.1 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C34 C32 C33 110.0(2) . . ?
C34 C32 P4 113.7(2) . . ?
C33 C32 P4 112.18(19) . . ?
C34 C32 H32 106.9 . . ?
C33 C32 H32 106.9 . . ?
P4 C32 H32 106.9 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C37 C35 C36 111.4(2) . . ?
C37 C35 P4 110.14(18) . . ?
C36 C35 P4 115.42(19) . . ?
C37 C35 H35 106.4 . . ?
C36 C35 H35 106.4 . . ?
P4 C35 H35 106.4 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N5 C38 H38A 109.5 . . ?
N5 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
N5 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N6 C39 H39A 109.5 . . ?
N6 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N6 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O2 C40 Mo2 175.4(2) . . ?

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
C20 Mo1 P1 N2 -135.39(11) . . . . ?
N1 Mo1 P1 N2 -17.77(10) . . . . ?
P2 Mo1 P1 N2 -66.55(9) . . . . ?
Br1 Mo1 P1 N2 146.67(8) . . . . ?
Br2 Mo1 P1 N2 56.13(8) . . . . ?
C20 Mo1 P1 C9 -17.15(13) . . . . ?
N1 Mo1 P1 C9 100.47(12) . . . . ?
P2 Mo1 P1 C9 51.69(11) . . . . ?
Br1 Mo1 P1 C9 -95.09(11) . . . . ?
Br2 Mo1 P1 C9 174.37(11) . . . . ?
C20 Mo1 P1 C6 112.12(12) . . . . ?
N1 Mo1 P1 C6 -130.26(11) . . . . ?
P2 Mo1 P1 C6 -179.05(10) . . . . ?
Br1 Mo1 P1 C6 34.18(10) . . . . ?
Br2 Mo1 P1 C6 -56.36(10) . . . . ?
C20 Mo1 P2 N3 150.36(11) . . . . ?
N1 Mo1 P2 N3 30.38(10) . . . . ?
P1 Mo1 P2 N3 80.04(9) . . . . ?
Br1 Mo1 P2 N3 -133.35(8) . . . . ?
Br2 Mo1 P2 N3 -43.44(8) . . . . ?
C20 Mo1 P2 C12 -96.21(12) . . . . ?
N1 Mo1 P2 C12 143.81(11) . . . . ?
P1 Mo1 P2 C12 -166.53(9) . . . . ?
Br1 Mo1 P2 C12 -19.92(10) . . . . ?
Br2 Mo1 P2 C12 69.99(9) . . . . ?
C20 Mo1 P2 C15 30.72(13) . . . . ?
N1 Mo1 P2 C15 -89.27(12) . . . . ?
P1 Mo1 P2 C15 -39.60(12) . . . . ?
Br1 Mo1 P2 C15 107.01(11) . . . . ?
Br2 Mo1 P2 C15 -163.08(11) . . . . ?
C40 Mo2 P3 N5 -152.03(12) . . . . ?
N4 Mo2 P3 N5 -31.48(10) . . . . ?
P4 Mo2 P3 N5 -81.40(9) . . . . ?
Br3 Mo2 P3 N5 132.06(8) . . . . ?
Br4 Mo2 P3 N5 41.76(8) . . . . ?
C40 Mo2 P3 C26 94.72(13) . . . . ?
N4 Mo2 P3 C26 -144.72(11) . . . . ?
P4 Mo2 P3 C26 165.36(10) . . . . ?
Br3 Mo2 P3 C26 18.82(10) . . . . ?
Br4 Mo2 P3 C26 -71.48(10) . . . . ?
C40 Mo2 P3 C29 -32.73(13) . . . . ?
N4 Mo2 P3 C29 87.82(12) . . . . ?
P4 Mo2 P3 C29 37.90(11) . . . . ?
Br3 Mo2 P3 C29 -108.64(11) . . . . ?
Br4 Mo2 P3 C29 161.06(11) . . . . ?
C40 Mo2 P4 N6 134.78(11) . . . . ?
N4 Mo2 P4 N6 16.79(10) . . . . ?
P3 Mo2 P4 N6 65.80(9) . . . . ?
Br3 Mo2 P4 N6 -147.81(8) . . . . ?
Br4 Mo2 P4 N6 -57.76(8) . . . . ?
C40 Mo2 P4 C35 15.90(13) . . . . ?
N4 Mo2 P4 C35 -102.09(12) . . . . ?
P3 Mo2 P4 C35 -53.08(12) . . . . ?
Br3 Mo2 P4 C35 93.31(11) . . . . ?
Br4 Mo2 P4 C35 -176.64(11) . . . . ?
C40 Mo2 P4 C32 -112.31(13) . . . . ?
N4 Mo2 P4 C32 129.70(12) . . . . ?
P3 Mo2 P4 C32 178.72(10) . . . . ?
Br3 Mo2 P4 C32 -34.90(11) . . . . ?
Br4 Mo2 P4 C32 55.15(10) . . . . ?
C20 Mo1 N1 C5 -96.4(2) . . . . ?
P2 Mo1 N1 C5 -28.16(17) . . . . ?
P1 Mo1 N1 C5 -169.88(19) . . . . ?
Br1 Mo1 N1 C5 77.7(3) . . . . ?
Br2 Mo1 N1 C5 80.27(18) . . . . ?
C20 Mo1 N1 C1 91.8(2) . . . . ?
P2 Mo1 N1 C1 160.00(19) . . . . ?
P1 Mo1 N1 C1 18.28(17) . . . . ?
Br1 Mo1 N1 C1 -94.1(3) . . . . ?
Br2 Mo1 N1 C1 -91.57(18) . . . . ?
C9 P1 N2 C1 -113.5(2) . . . . ?
C6 P1 N2 C1 140.2(2) . . . . ?
Mo1 P1 N2 C1 21.2(2) . . . . ?
C9 P1 N2 C18 56.0(2) . . . . ?
C6 P1 N2 C18 -50.3(2) . . . . ?
Mo1 P1 N2 C18 -169.30(19) . . . . ?
C12 P2 N3 C5 -156.35(18) . . . . ?
C15 P2 N3 C5 93.9(2) . . . . ?
Mo1 P2 N3 C5 -38.22(19) . . . . ?
C12 P2 N3 C19 44.9(2) . . . . ?
C15 P2 N3 C19 -64.9(2) . . . . ?
Mo1 P2 N3 C19 163.0(2) . . . . ?
C40 Mo2 N4 C21 96.6(2) . . . . ?
P3 Mo2 N4 C21 28.88(17) . . . . ?
P4 Mo2 N4 C21 170.19(19) . . . . ?
Br3 Mo2 N4 C21 -74.9(3) . . . . ?
Br4 Mo2 N4 C21 -81.39(18) . . . . ?
C40 Mo2 N4 C25 -90.9(2) . . . . ?
P3 Mo2 N4 C25 -158.59(19) . . . . ?
P4 Mo2 N4 C25 -17.29(17) . . . . ?
Br3 Mo2 N4 C25 97.7(3) . . . . ?
Br4 Mo2 N4 C25 91.14(18) . . . . ?
C26 P3 N5 C21 157.80(18) . . . . ?
C29 P3 N5 C21 -92.2(2) . . . . ?
Mo2 P3 N5 C21 39.73(19) . . . . ?
C26 P3 N5 C38 -44.7(2) . . . . ?
C29 P3 N5 C38 65.3(2) . . . . ?
Mo2 P3 N5 C38 -162.8(2) . . . . ?
C35 P4 N6 C25 114.9(2) . . . . ?
C32 P4 N6 C25 -139.3(2) . . . . ?
Mo2 P4 N6 C25 -20.0(2) . . . . ?
C35 P4 N6 C39 -56.2(2) . . . . ?
C32 P4 N6 C39 49.6(2) . . . . ?
Mo2 P4 N6 C39 168.95(19) . . . . ?
C5 N1 C1 N2 176.9(2) . . . . ?
Mo1 N1 C1 N2 -11.0(3) . . . . ?
C5 N1 C1 C2 -2.0(4) . . . . ?
Mo1 N1 C1 C2 170.11(19) . . . . ?
C18 N2 C1 N1 -178.4(2) . . . . ?
P1 N2 C1 N1 -8.4(3) . . . . ?
C18 N2 C1 C2 0.5(4) . . . . ?
P1 N2 C1 C2 170.5(2) . . . . ?
N1 C1 C2 C3 0.4(4) . . . . ?
N2 C1 C2 C3 -178.4(2) . . . . ?
C1 C2 C3 C4 0.4(4) . . . . ?
C2 C3 C4 C5 0.4(4) . . . . ?
C1 N1 C5 N3 -174.7(2) . . . . ?
Mo1 N1 C5 N3 13.1(3) . . . . ?
C1 N1 C5 C4 2.9(4) . . . . ?
Mo1 N1 C5 C4 -169.3(2) . . . . ?
C19 N3 C5 N1 179.3(2) . . . . ?
P2 N3 C5 N1 18.9(3) . . . . ?
C19 N3 C5 C4 1.6(4) . . . . ?
P2 N3 C5 C4 -158.8(2) . . . . ?
C3 C4 C5 N1 -2.1(4) . . . . ?
C3 C4 C5 N3 175.4(2) . . . . ?
N2 P1 C6 C8 -45.1(2) . . . . ?
C9 P1 C6 C8 -150.6(2) . . . . ?
Mo1 P1 C6 C8 68.2(2) . . . . ?
N2 P1 C6 C7 -170.71(19) . . . . ?
C9 P1 C6 C7 83.8(2) . . . . ?
Mo1 P1 C6 C7 -57.4(2) . . . . ?
N2 P1 C9 C11 67.7(2) . . . . ?
C6 P1 C9 C11 174.80(18) . . . . ?
Mo1 P1 C9 C11 -52.1(2) . . . . ?
N2 P1 C9 C10 -164.8(2) . . . . ?
C6 P1 C9 C10 -57.6(2) . . . . ?
Mo1 P1 C9 C10 75.5(2) . . . . ?
N3 P2 C12 C14 60.3(2) . . . . ?
C15 P2 C12 C14 170.87(19) . . . . ?
Mo1 P2 C12 C14 -51.8(2) . . . . ?
N3 P2 C12 C13 -174.51(18) . . . . ?
C15 P2 C12 C13 -63.9(2) . . . . ?
Mo1 P2 C12 C13 73.35(19) . . . . ?
N3 P2 C15 C17 71.7(2) . . . . ?
C12 P2 C15 C17 -39.2(2) . . . . ?
Mo1 P2 C15 C17 -169.48(16) . . . . ?
N3 P2 C15 C16 -52.5(2) . . . . ?
C12 P2 C15 C16 -163.32(19) . . . . ?
Mo1 P2 C15 C16 66.4(2) . . . . ?
C25 N4 C21 N5 174.1(2) . . . . ?
Mo2 N4 C21 N5 -13.1(3) . . . . ?
C25 N4 C21 C22 -3.5(4) . . . . ?
Mo2 N4 C21 C22 169.3(2) . . . . ?
C38 N5 C21 N4 -179.0(2) . . . . ?
P3 N5 C21 N4 -19.9(3) . . . . ?
C38 N5 C21 C22 -1.4(4) . . . . ?
P3 N5 C21 C22 157.8(2) . . . . ?
N4 C21 C22 C23 2.8(4) . . . . ?
N5 C21 C22 C23 -174.6(2) . . . . ?
C21 C22 C23 C24 -0.8(4) . . . . ?
C22 C23 C24 C25 -0.5(4) . . . . ?
C21 N4 C25 N6 -176.8(2) . . . . ?
Mo2 N4 C25 N6 10.5(3) . . . . ?
C21 N4 C25 C24 2.1(4) . . . . ?
Mo2 N4 C25 C24 -170.55(19) . . . . ?
C39 N6 C25 N4 179.3(2) . . . . ?
P4 N6 C25 N4 7.8(3) . . . . ?
C39 N6 C25 C24 0.3(4) . . . . ?
P4 N6 C25 C24 -171.1(2) . . . . ?
C23 C24 C25 N4 -0.2(4) . . . . ?
C23 C24 C25 N6 178.7(3) . . . . ?
N5 P3 C26 C27 174.47(18) . . . . ?
C29 P3 C26 C27 63.8(2) . . . . ?
Mo2 P3 C26 C27 -73.82(19) . . . . ?
N5 P3 C26 C28 -60.0(2) . . . . ?
C29 P3 C26 C28 -170.63(19) . . . . ?
Mo2 P3 C26 C28 51.8(2) . . . . ?
N5 P3 C29 C31 -71.3(2) . . . . ?
C26 P3 C29 C31 39.6(2) . . . . ?
Mo2 P3 C29 C31 170.37(16) . . . . ?
N5 P3 C29 C30 53.5(2) . . . . ?
C26 P3 C29 C30 164.41(19) . . . . ?
Mo2 P3 C29 C30 -64.8(2) . . . . ?
N6 P4 C32 C34 43.1(2) . . . . ?
C35 P4 C32 C34 148.7(2) . . . . ?
Mo2 P4 C32 C34 -70.8(2) . . . . ?
N6 P4 C32 C33 168.7(2) . . . . ?
C35 P4 C32 C33 -85.7(2) . . . . ?
Mo2 P4 C32 C33 54.8(2) . . . . ?
N6 P4 C35 C37 -67.1(2) . . . . ?
C32 P4 C35 C37 -174.33(19) . . . . ?
Mo2 P4 C35 C37 53.3(2) . . . . ?
N6 P4 C35 C36 165.6(2) . . . . ?
C32 P4 C35 C36 58.4(2) . . . . ?
Mo2 P4 C35 C36 -73.9(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.094
_refine_diff_density_min         -1.641
_refine_diff_density_rms         0.102

#===END



# start Validation Reply Form

_vrf_PLAT241_3-1697              
;
PROBLEM:
PLAT241_ALERT_2_C High Ueq as Compared to Neighbors for C35 Check
RESPONSE: 
The crystal structure contains two independent Mo complexes of similar
geometry and dimensions. While the first of these complexes is 
well ordered, the second shows some orientation disorder for two 
of its isopropyl groups next to the carbonyl group C40 O2.
This disorder was taken into account by refining split positions
C30A/C30B and C37A/C37B for two methyl carbon atoms.
;

_vrf_PLAT301_3-1697              
;
PROBLEM:     
PLAT301_ALERT_3_G Main Residue Disorder . Percentage = 3 Note
RESPONSE: 
See PLAT241_ALERT_2_C for explanation.
;

_vrf_PLAT601_4-1680              
;
PROBLEM:     
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 50 Ang3
RESPONSE: 
This structure and the isostructural chloride complex 5-1701 contain
relatively large voids in their crystal lattices which were found to be
unoccupied, however. It appears that both solids, 4-1680 and 5-1701,
are therefore prone to polymorph formation and for the Br-complex indeed a
second monoclinic polymorph with a unit cell twice as large as 4-1680
and two independent Mo complexes with significant difference in 
conformation was found (one of the four isopropyl groups turned about
the N-C bond by ca. 120 deg).
;

_vrf_PLAT601_5-1701              
;
PROBLEM:     
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 44 Ang3
RESPONSE: 
This structure and the isostructural bromide complex 4-1680 contain
relatively large voids in their crystal lattices which were found to be
unoccupied, however. It appears that both solids, 4-1680 and 5-1701,
are therefore prone to polymorph formation and for the Br-complex indeed a
second monoclinic polymorph with a unit cell twice as large as 4-1680
and two independent Mo complexes with a significant difference in 
conformation was found (one of the four isopropyl groups turned about
the N-C bond by ca. 120 deg).
;

_vrf_PLAT220_8-1703              
;
PROBLEM:     
Alert level B
PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.4 Ratio
RESPONSE: 
The fluorine atoms of the SbF6 group have relatively large displacement
parameters perpendicular to their SbF6 bonds indicating a common type
of disorder for XF6 groups. This disorder appears to affect to a lesser 
extent the carbonyl and the chloride ligand of the Mo complex and one 
isopropyl group.
;

_vrf_PLAT222_8-1703              
;
PROBLEM:     
Alert level C
PLAT222_ALERT_3_C Large Non-Solvent H Uiso(max)/Uiso(min) .. 4.3 Ratio
RESPONSE: 
See PLAT220_ALERT_2_B for explanation
;

_vrf_PLAT005_4b-1702             
;
PROBLEM:     
This G alert was used to give a special information. 
RESPONSE: 
This G alert was used to give a special information.
4b-1702 [Mo(PNP^Me^-iPr)(CO)Br2] is the second polymorph
of the complex [Mo(PNP^Me^-iPr)(CO)Br2] which has a 
higher density of 1.732 g/cm3 than the first polymorph
which is reported as 4-1680 [Mo(PNP^Me^-iPr)(CO)Br2]
in this CIF and which has a density 1.666 g/cm3.
It seems that 4-1680 is a kinetically favoured 
crystal form whereas 4b-1702 should be a thermodynamically
favoured form. Both forms were obtained in two independent 
experiments by crystallization with the solvent/antisolvent
vapour diffusion method using CH2Cl2/pentane and/or diethyl ether.
The [Mo(PNP^Me^-iPr)(CO)Br2] complexes
in both polymorphs are very similar in bond lengths,
bond angles and general conformation but differ in the 
orientation of one out of four isopropyl groups (C9,C10,C11). 
This isopropyl group has a torsion angle of 
Mo1-P1-C9-H9 = 42.3 deg in 4-1680 and 166.6 deg in 4b-1702,
(first complex in 4b-1702, the independent second complex in 4b-1702 
is very similar).
Due to inefficient packing the structure of 4-1680 contains 
solvent accessible voids of ca. 50 A^3^ (unoccupied, no solvent
electron density detected), whereas the structure of 4b-1702
has no solvent accessible voids.
;

# end Validation Reply Form

#=============================end of CIF======================================= 


_database_code_depnum_ccdc_archive 'CCDC 1004523'
