# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_I
_database_code_depnum_ccdc_archive 'CCDC 1983662'
_audit_update_record             
;
2020-02-12 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   14.6757(6)
_cell_length_b                   15.6115(6)
_cell_length_c                   21.3053(8)
_cell_angle_alpha                90
_cell_angle_beta                 109.233(2)
_cell_angle_gamma                90
_cell_volume                     4608.8(3)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mo -0.0483 2.7339 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584
4.3875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C43 H38 Cl2 Mo2 N6 O6 P2 
# Dc =      1.53 Fooo =   2136.00 Mu =     66.13 M =   1059.54
# Found Formula = C43 H38 Cl2 Mo2 N6 O6 P2 
# Dc =      1.53 FOOO =   2136.00 Mu =     66.13 M =   1059.54

_chemical_formula_sum            'C43 H38 Cl2 Mo2 N6 O6 P2'
_chemical_formula_moiety         'C42 H36 Mo2 N6 O6 P2, C H2 Cl2'
_chemical_compound_source        synthetic
_chemical_formula_weight         1059.54


_cell_measurement_reflns_used    9957
_cell_measurement_theta_min      3.58
_cell_measurement_theta_max      66.88
_cell_measurement_temperature    180

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.030
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_max          0.140

_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2136
_exptl_absorpt_coefficient_mu    6.613

# Sheldrick geometric approximatio 0.45 0.82 
# No experimental values of Tmin/max available 
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.5494
_exptl_absorpt_correction_T_max  0.7528
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω/2θ

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      180
_diffrn_reflns_number            8203
_reflns_number_total             8203
_diffrn_reflns_av_R_equivalents  0.000
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 8203 
# Theoretical number of reflections is about 16414 


_diffrn_reflns_theta_min         3.222
_diffrn_reflns_theta_max         66.946
_diffrn_measured_fraction_theta_max 0.997

_diffrn_reflns_theta_full        66.946
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       25
_reflns_limit_h_min              -17
_reflns_limit_h_max              16
_reflns_limit_k_min              0
_reflns_limit_k_max              18
_reflns_limit_l_min              0
_reflns_limit_l_max              25

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.94
_refine_diff_density_max         0.74


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_restraints     0
_refine_ls_number_parameters     550
_refine_ls_number_reflns         8165
_oxford_refine_ls_R_factor_ref   0.0483
_refine_ls_wR_factor_ref         0.0813
_refine_ls_goodness_of_fit_ref   0.9133
_refine_ls_shift/su_max          0.0017111
_refine_ls_shift/su_mean         0.0000394


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        8165
_refine_ls_R_factor_all          0.0483
_refine_ls_wR_factor_all         0.0813

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6813
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_gt          0.0757


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.182E+04 0.287E+04 0.166E+04 725. 188. 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mo1 Mo 0.30807(2) 0.79084(2) 0.685234(16) 0.0261 1.0000 Uani . . . . . .
Mo2 Mo 0.65961(2) 0.724025(18) 0.628156(14) 0.0170 1.0000 Uani . . . . . .
P1 P 0.50721(6) 0.77547(6) 0.64524(4) 0.0176 1.0000 Uani . . . . . .
P2 P 0.75484(6) 0.71049(6) 0.75336(5) 0.0190 1.0000 Uani . . . . . .
N1 N 0.4403(2) 0.8782(2) 0.72710(15) 0.0233 1.0000 Uani . . . . . .
N2 N 0.3241(2) 0.8344(2) 0.58394(15) 0.0216 1.0000 Uani . . . . . .
N3 N 0.3899(2) 0.6382(2) 0.61315(17) 0.0262 1.0000 Uani . . . . . .
N4 N 0.6460(2) 0.59593(19) 0.67855(15) 0.0206 1.0000 Uani . . . . . .
N5 N 0.9247(2) 0.6350(2) 0.82604(16) 0.0231 1.0000 Uani . . . . . .
N6 N 0.6565(2) 0.7443(2) 0.83753(16) 0.0269 1.0000 Uani . . . . . .
O1 O 0.1432(3) 0.6608(3) 0.6235(2) 0.0628 1.0000 Uani . . . . . .
O2 O 0.2876(3) 0.7448(4) 0.8209(2) 0.0820 1.0000 Uani . . . . . .
O3 O 0.1398(2) 0.9062(3) 0.69000(18) 0.0552 1.0000 Uani . . . . . .
O4 O 0.6990(2) 0.90638(19) 0.58485(16) 0.0391 1.0000 Uani . . . . . .
O5 O 0.5554(2) 0.6898(2) 0.47694(14) 0.0372 1.0000 Uani . . . . . .
O6 O 0.8339(3) 0.6501(3) 0.59117(19) 0.0623 1.0000 Uani . . . . . .
C1 C 0.5186(3) 0.8585(2) 0.70894(17) 0.0191 1.0000 Uani . . . . . .
C2 C 0.6051(3) 0.9019(2) 0.73327(19) 0.0239 1.0000 Uani . . . . . .
C3 C 0.6145(3) 0.9671(3) 0.7791(2) 0.0299 1.0000 Uani . . . . . .
C4 C 0.5364(3) 0.9876(3) 0.7973(2) 0.0331 1.0000 Uani . . . . . .
C5 C 0.4492(3) 0.9443(3) 0.7705(2) 0.0306 1.0000 Uani . . . . . .
C6 C 0.3644(4) 0.9705(4) 0.7896(3) 0.0493 1.0000 Uani . . . . . .
C7 C 0.4124(3) 0.8272(2) 0.57657(17) 0.0178 1.0000 Uani . . . . . .
C8 C 0.4342(3) 0.8595(2) 0.52324(19) 0.0228 1.0000 Uani . . . . . .
C9 C 0.3626(3) 0.9015(3) 0.47282(19) 0.0262 1.0000 Uani . . . . . .
C10 C 0.2728(3) 0.9073(3) 0.47927(19) 0.0270 1.0000 Uani . . . . . .
C11 C 0.2539(3) 0.8724(3) 0.53373(19) 0.0259 1.0000 Uani . . . . . .
C12 C 0.1532(3) 0.8769(4) 0.5359(2) 0.0456 1.0000 Uani . . . . . .
C13 C 0.4347(3) 0.6911(2) 0.66616(19) 0.0227 1.0000 Uani . . . . . .
C14 C 0.4449(3) 0.6713(3) 0.7313(2) 0.0292 1.0000 Uani . . . . . .
C15 C 0.4091(3) 0.5914(3) 0.7437(2) 0.0374 1.0000 Uani . . . . . .
C16 C 0.3646(3) 0.5393(3) 0.6920(2) 0.0376 1.0000 Uani . . . . . .
C17 C 0.3542(3) 0.5651(3) 0.6265(2) 0.0324 1.0000 Uani . . . . . .
C18 C 0.3035(4) 0.5078(3) 0.5688(3) 0.0493 1.0000 Uani . . . . . .
C19 C 0.6972(3) 0.6054(2) 0.74443(18) 0.0212 1.0000 Uani . . . . . .
C20 C 0.6996(3) 0.5442(3) 0.7908(2) 0.0257 1.0000 Uani . . . . . .
C21 C 0.6476(3) 0.4694(3) 0.7699(2) 0.0288 1.0000 Uani . . . . . .
C22 C 0.5984(3) 0.4581(3) 0.7031(2) 0.0281 1.0000 Uani . . . . . .
C23 C 0.6000(3) 0.5216(2) 0.65734(19) 0.0236 1.0000 Uani . . . . . .
C24 C 0.5536(3) 0.5093(3) 0.58389(19) 0.0311 1.0000 Uani . . . . . .
C25 C 0.8851(3) 0.6906(2) 0.77636(18) 0.0221 1.0000 Uani . . . . . .
C26 C 0.9368(3) 0.7344(3) 0.7432(2) 0.0305 1.0000 Uani . . . . . .
C27 C 1.0371(3) 0.7222(3) 0.7633(3) 0.0424 1.0000 Uani . . . . . .
C28 C 1.0778(3) 0.6657(3) 0.8141(2) 0.0396 1.0000 Uani . . . . . .
C29 C 1.0209(3) 0.6225(3) 0.8440(2) 0.0278 1.0000 Uani . . . . . .
C30 C 1.0633(3) 0.5592(3) 0.8990(2) 0.0406 1.0000 Uani . . . . . .
C31 C 0.7453(3) 0.7508(2) 0.83222(18) 0.0220 1.0000 Uani . . . . . .
C32 C 0.8225(3) 0.7872(2) 0.88110(19) 0.0246 1.0000 Uani . . . . . .
C33 C 0.8077(3) 0.8171(3) 0.9381(2) 0.0324 1.0000 Uani . . . . . .
C34 C 0.7184(3) 0.8108(3) 0.9443(2) 0.0351 1.0000 Uani . . . . . .
C35 C 0.6432(3) 0.7736(3) 0.8929(2) 0.0318 1.0000 Uani . . . . . .
C36 C 0.5437(4) 0.7644(4) 0.8976(2) 0.0547 1.0000 Uani . . . . . .
C37 C 0.2052(3) 0.7088(3) 0.6460(2) 0.0397 1.0000 Uani . . . . . .
C38 C 0.2972(3) 0.7600(4) 0.7711(2) 0.0456 1.0000 Uani . . . . . .
C39 C 0.2052(3) 0.8668(3) 0.6856(2) 0.0366 1.0000 Uani . . . . . .
C40 C 0.6849(3) 0.8383(3) 0.60145(19) 0.0251 1.0000 Uani . . . . . .
C41 C 0.5913(3) 0.7016(2) 0.5337(2) 0.0248 1.0000 Uani . . . . . .
C42 C 0.7725(3) 0.6780(3) 0.6075(2) 0.0338 1.0000 Uani . . . . . .
Cl2 Cl 0.35748(18) 0.60170(19) 0.93884(13) 0.1207 1.0000 Uani . . . . . .
Cl1 Cl 0.43453(15) 0.6266(3) 1.07866(14) 0.1817 1.0000 Uani . . . . . .
C100 C 0.3487(7) 0.6614(8) 0.9997(5) 0.1421 1.0000 Uani . . . . . .
H21 H 0.6555 0.8873 0.7180 0.0293 1.0000 Uiso R . . . . .
H31 H 0.6723 0.9960 0.7967 0.0362 1.0000 Uiso R . . . . .
H41 H 0.5412 1.0303 0.8279 0.0398 1.0000 Uiso R . . . . .
H62 H 0.3408 0.9227 0.8072 0.0739 1.0000 Uiso R . . . . .
H61 H 0.3833 1.0148 0.8220 0.0743 1.0000 Uiso R . . . . .
H63 H 0.3149 0.9911 0.7505 0.0737 1.0000 Uiso R . . . . .
H81 H 0.4957 0.8536 0.5206 0.0267 1.0000 Uiso R . . . . .
H91 H 0.3762 0.9242 0.4366 0.0312 1.0000 Uiso R . . . . .
H101 H 0.2241 0.9349 0.4469 0.0321 1.0000 Uiso R . . . . .
H121 H 0.1351 0.8235 0.5508 0.0682 1.0000 Uiso R . . . . .
H123 H 0.1494 0.9209 0.5669 0.0680 1.0000 Uiso R . . . . .
H122 H 0.1083 0.8909 0.4929 0.0681 1.0000 Uiso R . . . . .
H141 H 0.4972 0.6967 0.7666 0.0352 1.0000 Uiso R . . . . .
H151 H 0.4157 0.5751 0.7868 0.0452 1.0000 Uiso R . . . . .
H161 H 0.3424 0.4863 0.6994 0.0454 1.0000 Uiso R . . . . .
H182 H 0.3147 0.5269 0.5294 0.0741 1.0000 Uiso R . . . . .
H183 H 0.2363 0.5079 0.5623 0.0743 1.0000 Uiso R . . . . .
H181 H 0.3269 0.4506 0.5787 0.0737 1.0000 Uiso R . . . . .
H201 H 0.7358 0.5527 0.8348 0.0306 1.0000 Uiso R . . . . .
H211 H 0.6447 0.4282 0.7999 0.0348 1.0000 Uiso R . . . . .
H221 H 0.5642 0.4080 0.6884 0.0339 1.0000 Uiso R . . . . .
H242 H 0.5075 0.5545 0.5669 0.0470 1.0000 Uiso R . . . . .
H243 H 0.6017 0.5100 0.5622 0.0465 1.0000 Uiso R . . . . .
H241 H 0.5198 0.4559 0.5754 0.0470 1.0000 Uiso R . . . . .
H261 H 0.9057 0.7716 0.7087 0.0368 1.0000 Uiso R . . . . .
H271 H 1.0749 0.7518 0.7430 0.0507 1.0000 Uiso R . . . . .
H281 H 1.1439 0.6565 0.8287 0.0482 1.0000 Uiso R . . . . .
H301 H 1.0148 0.5209 0.9035 0.0609 1.0000 Uiso R . . . . .
H302 H 1.0897 0.5894 0.9394 0.0613 1.0000 Uiso R . . . . .
H303 H 1.1137 0.5266 0.8912 0.0612 1.0000 Uiso R . . . . .
H321 H 0.8819 0.7909 0.8756 0.0298 1.0000 Uiso R . . . . .
H331 H 0.8572 0.8420 0.9719 0.0390 1.0000 Uiso R . . . . .
H341 H 0.7065 0.8310 0.9816 0.0418 1.0000 Uiso R . . . . .
H363 H 0.5234 0.7065 0.8906 0.0817 1.0000 Uiso R . . . . .
H361 H 0.4987 0.7989 0.8641 0.0820 1.0000 Uiso R . . . . .
H362 H 0.5426 0.7824 0.9401 0.0819 1.0000 Uiso R . . . . .
H1001 H 0.3617 0.7199 0.9914 0.1700 1.0000 Uiso R . . . . .
H1002 H 0.2841 0.6572 1.0019 0.1700 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.370(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mo1 . N1 . 2.298(3) yes
Mo1 . N2 . 2.347(3) yes
Mo1 . C13 . 2.557(4) yes
Mo1 . C14 . 2.680(4) yes
Mo1 . C37 . 1.946(5) yes
Mo1 . C38 . 1.948(5) yes
Mo1 . C39 . 1.921(5) yes
Mo2 . P1 . 2.5132(9) yes
Mo2 . P2 . 2.5801(9) yes
Mo2 . N4 . 2.309(3) yes
Mo2 . C40 . 1.945(4) yes
Mo2 . C41 . 1.961(4) yes
Mo2 . C42 . 1.985(5) yes
P1 . C1 . 1.844(4) yes
P1 . C7 . 1.841(4) yes
P1 . C13 . 1.838(4) yes
P2 . C19 . 1.827(4) yes
P2 . C25 . 1.837(4) yes
P2 . C31 . 1.842(4) yes
N1 . C1 . 1.363(5) yes
N1 . C5 . 1.364(5) yes
N2 . C7 . 1.361(5) yes
N2 . C11 . 1.353(5) yes
N3 . C13 . 1.379(5) yes
N3 . C17 . 1.325(5) yes
N4 . C19 . 1.364(5) yes
N4 . C23 . 1.343(5) yes
N5 . C25 . 1.344(5) yes
N5 . C29 . 1.349(5) yes
N6 . C31 . 1.348(5) yes
N6 . C35 . 1.337(5) yes
O1 . C37 . 1.154(6) yes
O2 . C38 . 1.141(6) yes
O3 . C39 . 1.169(5) yes
O4 . C40 . 1.160(5) yes
O5 . C41 . 1.164(5) yes
O6 . C42 . 1.151(5) yes
C1 . C2 . 1.381(5) yes
C2 . C3 . 1.386(6) yes
C2 . H21 . 0.928 no
C3 . C4 . 1.363(6) yes
C3 . H31 . 0.923 no
C4 . C5 . 1.392(6) yes
C4 . H41 . 0.920 no
C5 . C6 . 1.488(6) yes
C6 . H62 . 0.951 no
C6 . H61 . 0.953 no
C6 . H63 . 0.962 no
C7 . C8 . 1.374(5) yes
C8 . C9 . 1.395(5) yes
C8 . H81 . 0.927 no
C9 . C10 . 1.372(6) yes
C9 . H91 . 0.929 no
C10 . C11 . 1.390(6) yes
C10 . H101 . 0.920 no
C11 . C12 . 1.497(6) yes
C12 . H121 . 0.960 no
C12 . H123 . 0.967 no
C12 . H122 . 0.961 no
C13 . C14 . 1.381(6) yes
C14 . C15 . 1.412(6) yes
C14 . H141 . 0.966 no
C15 . C16 . 1.351(7) yes
C15 . H151 . 0.926 no
C16 . C17 . 1.413(6) yes
C16 . H161 . 0.922 no
C17 . C18 . 1.504(6) yes
C18 . H182 . 0.954 no
C18 . H183 . 0.949 no
C18 . H181 . 0.954 no
C19 . C20 . 1.366(5) yes
C20 . C21 . 1.386(6) yes
C20 . H201 . 0.923 no
C21 . C22 . 1.379(6) yes
C21 . H211 . 0.917 no
C22 . C23 . 1.397(6) yes
C22 . H221 . 0.927 no
C23 . C24 . 1.499(5) yes
C24 . H242 . 0.961 no
C24 . H243 . 0.963 no
C24 . H241 . 0.957 no
C25 . C26 . 1.376(6) yes
C26 . C27 . 1.404(6) yes
C26 . H261 . 0.930 no
C27 . C28 . 1.371(7) yes
C27 . H271 . 0.932 no
C28 . C29 . 1.382(6) yes
C28 . H281 . 0.927 no
C29 . C30 . 1.502(6) yes
C30 . H301 . 0.957 no
C30 . H302 . 0.946 no
C30 . H303 . 0.957 no
C31 . C32 . 1.383(5) yes
C32 . C33 . 1.383(6) yes
C32 . H321 . 0.920 no
C33 . C34 . 1.364(6) yes
C33 . H331 . 0.923 no
C34 . C35 . 1.400(6) yes
C34 . H341 . 0.924 no
C35 . C36 . 1.504(6) yes
C36 . H363 . 0.949 no
C36 . H361 . 0.962 no
C36 . H362 . 0.952 no
Cl2 . C100 . 1.637(10) yes
Cl1 . C100 . 1.821(11) yes
C100 . H1001 . 0.962 no
C100 . H1002 . 0.965 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Mo1 . N2 . 81.80(11) yes
N1 . Mo1 . C13 . 81.83(11) yes
N2 . Mo1 . C13 . 74.47(11) yes
N1 . Mo1 . C14 . 80.56(12) yes
N2 . Mo1 . C14 . 104.40(12) yes
C13 . Mo1 . C14 . 30.46(12) yes
N1 . Mo1 . C37 . 173.56(16) yes
N2 . Mo1 . C37 . 95.40(16) yes
C13 . Mo1 . C37 . 91.85(16) yes
C14 . Mo1 . C37 . 94.60(16) yes
N1 . Mo1 . C38 . 95.85(17) yes
N2 . Mo1 . C38 . 177.24(19) yes
C13 . Mo1 . C38 . 106.71(18) yes
C14 . Mo1 . C38 . 76.55(18) yes
C37 . Mo1 . C38 . 87.1(2) yes
N1 . Mo1 . C39 . 101.33(16) yes
N2 . Mo1 . C39 . 98.14(16) yes
C13 . Mo1 . C39 . 171.59(16) yes
C14 . Mo1 . C39 . 157.41(17) yes
C37 . Mo1 . C39 . 84.78(19) yes
C38 . Mo1 . C39 . 80.9(2) yes
P1 . Mo2 . P2 . 94.66(3) yes
P1 . Mo2 . N4 . 89.55(8) yes
P2 . Mo2 . N4 . 63.18(8) yes
P1 . Mo2 . C40 . 90.82(11) yes
P2 . Mo2 . C40 . 106.67(11) yes
N4 . Mo2 . C40 . 169.84(13) yes
P1 . Mo2 . C41 . 91.54(11) yes
P2 . Mo2 . C41 . 164.95(11) yes
N4 . Mo2 . C41 . 103.24(13) yes
C40 . Mo2 . C41 . 86.90(16) yes
P1 . Mo2 . C42 . 174.87(13) yes
P2 . Mo2 . C42 . 89.56(12) yes
N4 . Mo2 . C42 . 89.76(15) yes
C40 . Mo2 . C42 . 90.76(17) yes
C41 . Mo2 . C42 . 83.67(16) yes
Mo2 . P1 . C1 . 117.50(12) yes
Mo2 . P1 . C7 . 120.07(12) yes
C1 . P1 . C7 . 97.95(16) yes
Mo2 . P1 . C13 . 114.84(13) yes
C1 . P1 . C13 . 104.17(17) yes
C7 . P1 . C13 . 99.23(16) yes
Mo2 . P2 . C19 . 83.77(12) yes
Mo2 . P2 . C25 . 116.83(13) yes
C19 . P2 . C25 . 106.35(17) yes
Mo2 . P2 . C31 . 137.47(12) yes
C19 . P2 . C31 . 103.30(17) yes
C25 . P2 . C31 . 101.50(17) yes
Mo1 . N1 . C1 . 116.1(2) yes
Mo1 . N1 . C5 . 126.3(3) yes
C1 . N1 . C5 . 117.5(3) yes
Mo1 . N2 . C7 . 118.0(2) yes
Mo1 . N2 . C11 . 125.0(3) yes
C7 . N2 . C11 . 116.8(3) yes
C13 . N3 . C17 . 117.2(4) yes
Mo2 . N4 . C19 . 106.4(2) yes
Mo2 . N4 . C23 . 134.6(2) yes
C19 . N4 . C23 . 119.0(3) yes
C25 . N5 . C29 . 117.3(3) yes
C31 . N6 . C35 . 118.3(3) yes
P1 . C1 . N1 . 119.1(3) yes
P1 . C1 . C2 . 118.1(3) yes
N1 . C1 . C2 . 122.7(3) yes
C1 . C2 . C3 . 119.4(4) yes
C1 . C2 . H21 . 119.1 no
C3 . C2 . H21 . 121.5 no
C2 . C3 . C4 . 118.3(4) yes
C2 . C3 . H31 . 120.6 no
C4 . C3 . H31 . 121.1 no
C3 . C4 . C5 . 121.1(4) yes
C3 . C4 . H41 . 119.7 no
C5 . C4 . H41 . 119.2 no
C4 . C5 . N1 . 120.9(4) yes
C4 . C5 . C6 . 119.6(4) yes
N1 . C5 . C6 . 119.4(4) yes
C5 . C6 . H62 . 109.7 no
C5 . C6 . H61 . 109.1 no
H62 . C6 . H61 . 109.9 no
C5 . C6 . H63 . 108.4 no
H62 . C6 . H63 . 109.6 no
H61 . C6 . H63 . 110.0 no
P1 . C7 . N2 . 116.4(3) yes
P1 . C7 . C8 . 119.8(3) yes
N2 . C7 . C8 . 123.8(3) yes
C7 . C8 . C9 . 119.2(4) yes
C7 . C8 . H81 . 120.8 no
C9 . C8 . H81 . 120.1 no
C8 . C9 . C10 . 117.3(4) yes
C8 . C9 . H91 . 120.4 no
C10 . C9 . H91 . 122.3 no
C9 . C10 . C11 . 121.3(4) yes
C9 . C10 . H101 . 119.4 no
C11 . C10 . H101 . 119.3 no
C10 . C11 . N2 . 121.6(4) yes
C10 . C11 . C12 . 118.6(4) yes
N2 . C11 . C12 . 119.9(4) yes
C11 . C12 . H121 . 110.7 no
C11 . C12 . H123 . 109.5 no
H121 . C12 . H123 . 107.9 no
C11 . C12 . H122 . 110.7 no
H121 . C12 . H122 . 109.6 no
H123 . C12 . H122 . 108.4 no
P1 . C13 . N3 . 112.9(3) yes
P1 . C13 . Mo1 . 96.40(16) yes
N3 . C13 . Mo1 . 108.6(2) yes
P1 . C13 . C14 . 121.6(3) yes
N3 . C13 . C14 . 123.6(4) yes
Mo1 . C13 . C14 . 79.7(2) yes
C13 . C14 . Mo1 . 69.9(2) yes
C13 . C14 . C15 . 117.6(4) yes
Mo1 . C14 . C15 . 113.8(3) yes
C13 . C14 . H141 . 119.1 no
Mo1 . C14 . H141 . 107.9 no
C15 . C14 . H141 . 117.8 no
C14 . C15 . C16 . 119.3(4) yes
C14 . C15 . H151 . 120.3 no
C16 . C15 . H151 . 120.5 no
C15 . C16 . C17 . 120.0(4) yes
C15 . C16 . H161 . 120.3 no
C17 . C16 . H161 . 119.6 no
C16 . C17 . N3 . 122.4(4) yes
C16 . C17 . C18 . 120.1(4) yes
N3 . C17 . C18 . 117.5(4) yes
C17 . C18 . H182 . 110.5 no
C17 . C18 . H183 . 109.2 no
H182 . C18 . H183 . 110.1 no
C17 . C18 . H181 . 109.3 no
H182 . C18 . H181 . 109.4 no
H183 . C18 . H181 . 108.4 no
P2 . C19 . N4 . 106.4(3) yes
P2 . C19 . C20 . 130.7(3) yes
N4 . C19 . C20 . 122.8(3) yes
C19 . C20 . C21 . 118.5(4) yes
C19 . C20 . H201 . 120.2 no
C21 . C20 . H201 . 121.2 no
C20 . C21 . C22 . 118.9(4) yes
C20 . C21 . H211 . 121.0 no
C22 . C21 . H211 . 120.1 no
C21 . C22 . C23 . 120.5(4) yes
C21 . C22 . H221 . 119.9 no
C23 . C22 . H221 . 119.6 no
C22 . C23 . N4 . 120.0(3) yes
C22 . C23 . C24 . 122.1(3) yes
N4 . C23 . C24 . 117.8(3) yes
C23 . C24 . H242 . 108.7 no
C23 . C24 . H243 . 110.3 no
H242 . C24 . H243 . 110.3 no
C23 . C24 . H241 . 109.8 no
H242 . C24 . H241 . 108.1 no
H243 . C24 . H241 . 109.6 no
P2 . C25 . N5 . 117.5(3) yes
P2 . C25 . C26 . 118.7(3) yes
N5 . C25 . C26 . 123.8(4) yes
C25 . C26 . C27 . 118.4(4) yes
C25 . C26 . H261 . 120.4 no
C27 . C26 . H261 . 121.2 no
C26 . C27 . C28 . 118.0(4) yes
C26 . C27 . H271 . 121.0 no
C28 . C27 . H271 . 121.0 no
C27 . C28 . C29 . 120.3(4) yes
C27 . C28 . H281 . 120.0 no
C29 . C28 . H281 . 119.6 no
C28 . C29 . N5 . 122.2(4) yes
C28 . C29 . C30 . 121.5(4) yes
N5 . C29 . C30 . 116.3(4) yes
C29 . C30 . H301 . 111.0 no
C29 . C30 . H302 . 108.8 no
H301 . C30 . H302 . 108.5 no
C29 . C30 . H303 . 111.0 no
H301 . C30 . H303 . 109.1 no
H302 . C30 . H303 . 108.4 no
P2 . C31 . N6 . 114.6(3) yes
P2 . C31 . C32 . 122.5(3) yes
N6 . C31 . C32 . 122.8(4) yes
C31 . C32 . C33 . 118.3(4) yes
C31 . C32 . H321 . 120.4 no
C33 . C32 . H321 . 121.3 no
C32 . C33 . C34 . 119.6(4) yes
C32 . C33 . H331 . 121.2 no
C34 . C33 . H331 . 119.2 no
C33 . C34 . C35 . 119.3(4) yes
C33 . C34 . H341 . 121.2 no
C35 . C34 . H341 . 119.5 no
C34 . C35 . N6 . 121.7(4) yes
C34 . C35 . C36 . 121.3(4) yes
N6 . C35 . C36 . 117.0(4) yes
C35 . C36 . H363 . 109.9 no
C35 . C36 . H361 . 110.0 no
H363 . C36 . H361 . 108.3 no
C35 . C36 . H362 . 110.9 no
H363 . C36 . H362 . 109.2 no
H361 . C36 . H362 . 108.5 no
Mo1 . C37 . O1 . 178.6(5) yes
Mo1 . C38 . O2 . 176.9(5) yes
O3 . C39 . Mo1 . 172.5(4) yes
O4 . C40 . Mo2 . 179.1(3) yes
Mo2 . C41 . O5 . 176.1(3) yes
Mo2 . C42 . O6 . 175.3(4) yes
Cl1 . C100 . Cl2 . 110.5(6) yes
Cl1 . C100 . H1001 . 109.6 no
Cl2 . C100 . H1001 . 108.8 no
Cl1 . C100 . H1002 . 109.1 no
Cl2 . C100 . H1002 . 109.5 no
H1001 . C100 . H1002 . 109.3 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C14 . H141 . N6 . 164 0.97 2.44 3.382(6) yes
C28 . H281 . O2 1_655 133 0.93 2.57 3.276(6) yes


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
# SQUEEZE RESULTS (Version =  30118)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.500 124 39 ' '
2 0.205 0.794 0.918 11 0 ' '
3 0.301 0.291 0.583 9 0 ' '
4 0.502 1.001 1.001 123 39 ' '
5 0.699 0.709 0.417 10 0 ' '
6 0.801 0.209 0.083 9 0 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_added_by_encifer
_database_code_depnum_ccdc_archive 'CCDC 1983664'
_audit_update_record             
;
2020-02-12 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;
#------------------------------------------------------------------------------- 
# this cif originates from: 
#------------------------------------------------------------------------------- 
# leipzig university, faculty of chemistry and mineralogy, 
# johannisallee 29, 04103 leipzig, germany 
#------------------------------------------------------------------------------- 

#=============================================================================== 
#_leipzig_data_id data_x2857
#===============================================================================  

_audit_creation_method           
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H18 Mo N3 O5 P'
_chemical_formula_sum            'C23 H18 Mo N3 O5 P'
_chemical_formula_weight         543.31

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   10.4126(3)
_cell_length_b                   22.0156(5)
_cell_length_c                   10.8107(3)
_cell_angle_alpha                90
_cell_angle_beta                 109.128(3)
_cell_angle_gamma                90
_cell_volume                     2341.41(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    130.00(10)
_cell_measurement_reflns_used    8659
_cell_measurement_theta_min      2.9880
_cell_measurement_theta_max      32.0860

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_F_000             1096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.1500
_exptl_absorpt_coefficient_mu    0.667
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98637
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      130.00(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3560
_diffrn_reflns_number            20609
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.198
_diffrn_reflns_theta_max         32.587
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7736
_reflns_number_gt                6342
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 4'
_computing_publication_material  SHELXL

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0211P)²+1.4828P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7736
_refine_ls_number_parameters     301
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.0698
_refine_ls_wR_factor_gt          0.0649
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.33532(2) 0.67777(2) 0.81688(2) 0.01740(4) Uani 1 1 d . . . . .
P1 P 0.41492(4) 0.60253(2) 0.68380(4) 0.01559(8) Uani 1 1 d . . . . .
O1 O 0.62338(16) 0.68751(7) 1.04174(14) 0.0349(3) Uani 1 1 d . . . . .
O2 O 0.24747(17) 0.57031(7) 0.96828(15) 0.0359(4) Uani 1 1 d . . . . .
O3 O 0.05071(15) 0.67455(7) 0.58561(15) 0.0367(3) Uani 1 1 d . . . . .
O4 O 0.44318(16) 0.78856(7) 0.68739(16) 0.0351(3) Uani 1 1 d . . . . .
O5 O 0.21047(19) 0.77216(8) 0.96403(17) 0.0471(4) Uani 1 1 d . . . . .
N1 N 0.23393(14) 0.51447(7) 0.66872(14) 0.0181(3) Uani 1 1 d . . . . .
N2 N 0.35293(17) 0.67478(7) 0.47667(15) 0.0237(3) Uani 1 1 d . . . . .
N3 N 0.67247(15) 0.58849(7) 0.83624(14) 0.0191(3) Uani 1 1 d . . . . .
C1 C 0.36891(17) 0.52305(8) 0.69997(16) 0.0164(3) Uani 1 1 d . . . . .
C2 C 0.46330(18) 0.47691(8) 0.74362(19) 0.0229(4) Uani 1 1 d . . . . .
H2 H 0.5559 0.4847 0.7660 0.028 Uiso 1 1 calc R U . . .
C3 C 0.4159(2) 0.41887(9) 0.7530(2) 0.0276(4) Uani 1 1 d . . . . .
H3 H 0.4764 0.3868 0.7815 0.033 Uiso 1 1 calc R U . . .
C4 C 0.27798(19) 0.40928(8) 0.71962(19) 0.0236(4) Uani 1 1 d . . . . .
H4 H 0.2445 0.3705 0.7246 0.028 Uiso 1 1 calc R U . . .
C5 C 0.18871(17) 0.45830(8) 0.67820(15) 0.0180(3) Uani 1 1 d . . . . .
C6 C 0.03898(18) 0.44934(9) 0.64269(19) 0.0256(4) Uani 1 1 d . . . . .
H00A H -0.0020 0.4507 0.5492 0.038 Uiso 1 1 calc R U . . .
H00B H 0.0014 0.4809 0.6815 0.038 Uiso 1 1 calc R U . . .
H00C H 0.0212 0.4106 0.6745 0.038 Uiso 1 1 calc R U . . .
C7 C 0.34589(17) 0.61575(8) 0.50667(17) 0.0185(3) Uani 1 1 d . . . . .
C8 C 0.29492(17) 0.57127(8) 0.41339(17) 0.0200(3) Uani 1 1 d . . . . .
H8 H 0.2932 0.5308 0.4375 0.024 Uiso 1 1 calc R U . . .
C9 C 0.24630(18) 0.58854(9) 0.28264(18) 0.0235(4) Uani 1 1 d . . . . .
H9 H 0.2097 0.5598 0.2175 0.028 Uiso 1 1 calc R U . . .
C10 C 0.2530(2) 0.64870(10) 0.25069(18) 0.0264(4) Uani 1 1 d . . . . .
H10 H 0.2210 0.6611 0.1637 0.032 Uiso 1 1 calc R U . . .
C11 C 0.3082(2) 0.69094(9) 0.35003(19) 0.0275(4) Uani 1 1 d . . . . .
C12 C 0.3213(3) 0.75688(10) 0.3215(2) 0.0448(6) Uani 1 1 d . . . . .
H00I H 0.2390 0.7706 0.2570 0.067 Uiso 1 1 calc R U . . .
H00J H 0.3960 0.7622 0.2890 0.067 Uiso 1 1 calc R U . . .
H00L H 0.3374 0.7801 0.4004 0.067 Uiso 1 1 calc R U . . .
C13 C 0.59810(17) 0.59760(8) 0.71025(17) 0.0171(3) Uani 1 1 d . . . . .
C14 C 0.65441(18) 0.60287(8) 0.61062(17) 0.0212(3) Uani 1 1 d . . . . .
H14 H 0.5999 0.6094 0.5244 0.025 Uiso 1 1 calc R U . . .
C15 C 0.79489(19) 0.59801(9) 0.64381(19) 0.0251(4) Uani 1 1 d . . . . .
H15 H 0.8363 0.6016 0.5799 0.030 Uiso 1 1 calc R U . . .
C16 C 0.87178(19) 0.58785(9) 0.77253(19) 0.0245(4) Uani 1 1 d . . . . .
H16 H 0.9657 0.5839 0.7962 0.029 Uiso 1 1 calc R U . . .
C17 C 0.80757(18) 0.58349(8) 0.86717(18) 0.0212(3) Uani 1 1 d . . . . .
C18 C 0.8870(2) 0.57430(10) 1.00934(19) 0.0294(4) Uani 1 1 d . . . . .
H00D H 0.9786 0.5630 1.0182 0.044 Uiso 1 1 calc R U . . .
H00G H 0.8455 0.5427 1.0444 0.044 Uiso 1 1 calc R U . . .
H00H H 0.8876 0.6114 1.0563 0.044 Uiso 1 1 calc R U . . .
C19 C 0.5213(2) 0.68209(8) 0.96110(18) 0.0231(4) Uani 1 1 d . . . . .
C20 C 0.27895(19) 0.60834(9) 0.91257(18) 0.0239(4) Uani 1 1 d . . . . .
C21 C 0.15238(19) 0.67538(9) 0.66838(19) 0.0235(4) Uani 1 1 d . . . . .
C22 C 0.40225(19) 0.74800(8) 0.72766(19) 0.0233(4) Uani 1 1 d . . . . .
C23 C 0.2581(2) 0.73786(9) 0.9123(2) 0.0290(4) 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 C23 2.001(2) . ?
Mo1 C20 2.0369(19) . ?
Mo1 C21 2.0505(19) . ?
Mo1 C19 2.052(2) . ?
Mo1 C22 2.0610(19) . ?
Mo1 P1 2.5064(5) . ?
P1 C7 1.8347(17) . ?
P1 C13 1.8369(17) . ?
P1 C1 1.8375(17) . ?
O1 C19 1.139(2) . ?
O2 C20 1.140(2) . ?
O3 C21 1.141(2) . ?
O4 C22 1.136(2) . ?
O5 C23 1.145(2) . ?
N1 C5 1.339(2) . ?
N1 C1 1.347(2) . ?
N2 C11 1.342(2) . ?
N2 C7 1.347(2) . ?
N3 C17 1.340(2) . ?
N3 C13 1.343(2) . ?
C1 C2 1.384(2) . ?
C2 C3 1.386(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.377(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.399(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.492(2) . ?
C6 H00A 0.9600 . ?
C6 H00B 0.9600 . ?
C6 H00C 0.9600 . ?
C7 C8 1.381(2) . ?
C8 C9 1.389(2) . ?
C8 H8 0.9300 . ?
C9 C10 1.376(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.394(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.499(3) . ?
C12 H00I 0.9600 . ?
C12 H00J 0.9600 . ?
C12 H00L 0.9600 . ?
C13 C14 1.390(2) . ?
C14 C15 1.391(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.377(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.397(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.501(3) . ?
C18 H00D 0.9600 . ?
C18 H00G 0.9600 . ?
C18 H00H 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C23 Mo1 C20 90.18(8) . . ?
C23 Mo1 C21 89.63(8) . . ?
C20 Mo1 C21 91.72(7) . . ?
C23 Mo1 C19 90.93(8) . . ?
C20 Mo1 C19 90.35(7) . . ?
C21 Mo1 C19 177.85(7) . . ?
C23 Mo1 C22 89.99(8) . . ?
C20 Mo1 C22 176.98(8) . . ?
C21 Mo1 C22 91.30(7) . . ?
C19 Mo1 C22 86.63(7) . . ?
C23 Mo1 P1 175.66(6) . . ?
C20 Mo1 P1 90.01(5) . . ?
C21 Mo1 P1 86.03(5) . . ?
C19 Mo1 P1 93.41(5) . . ?
C22 Mo1 P1 90.06(5) . . ?
C7 P1 C13 101.74(8) . . ?
C7 P1 C1 103.01(8) . . ?
C13 P1 C1 102.63(8) . . ?
C7 P1 Mo1 113.84(6) . . ?
C13 P1 Mo1 118.13(6) . . ?
C1 P1 Mo1 115.41(5) . . ?
C5 N1 C1 118.33(15) . . ?
C11 N2 C7 118.26(17) . . ?
C17 N3 C13 118.34(15) . . ?
N1 C1 C2 123.26(16) . . ?
N1 C1 P1 113.13(12) . . ?
C2 C1 P1 123.58(13) . . ?
C1 C2 C3 118.12(17) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
C4 C3 C2 119.22(18) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 119.47(17) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 121.57(16) . . ?
N1 C5 C6 117.81(16) . . ?
C4 C5 C6 120.62(16) . . ?
C5 C6 H00A 109.5 . . ?
C5 C6 H00B 109.5 . . ?
H00A C6 H00B 109.5 . . ?
C5 C6 H00C 109.5 . . ?
H00A C6 H00C 109.5 . . ?
H00B C6 H00C 109.5 . . ?
N2 C7 C8 123.13(16) . . ?
N2 C7 P1 111.76(13) . . ?
C8 C7 P1 125.10(14) . . ?
C7 C8 C9 118.28(17) . . ?
C7 C8 H8 120.9 . . ?
C9 C8 H8 120.9 . . ?
C10 C9 C8 119.15(18) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C9 C10 C11 119.38(17) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
N2 C11 C10 121.78(18) . . ?
N2 C11 C12 116.23(19) . . ?
C10 C11 C12 121.99(18) . . ?
C11 C12 H00I 109.5 . . ?
C11 C12 H00J 109.5 . . ?
H00I C12 H00J 109.5 . . ?
C11 C12 H00L 109.5 . . ?
H00I C12 H00L 109.5 . . ?
H00J C12 H00L 109.5 . . ?
N3 C13 C14 123.29(16) . . ?
N3 C13 P1 113.01(12) . . ?
C14 C13 P1 123.69(13) . . ?
C13 C14 C15 117.94(17) . . ?
C13 C14 H14 121.0 . . ?
C15 C14 H14 121.0 . . ?
C16 C15 C14 119.14(16) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C15 C16 C17 119.46(17) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
N3 C17 C16 121.81(17) . . ?
N3 C17 C18 116.60(16) . . ?
C16 C17 C18 121.58(16) . . ?
C17 C18 H00D 109.5 . . ?
C17 C18 H00G 109.5 . . ?
H00D C18 H00G 109.5 . . ?
C17 C18 H00H 109.5 . . ?
H00D C18 H00H 109.5 . . ?
H00G C18 H00H 109.5 . . ?
O1 C19 Mo1 176.56(17) . . ?
O2 C20 Mo1 178.53(16) . . ?
O3 C21 Mo1 179.44(17) . . ?
O4 C22 Mo1 174.94(17) . . ?
O5 C23 Mo1 178.0(2) . . ?

_refine_diff_density_max         0.424
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.076

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_added_by_encifer_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1983665'
_audit_update_record             
;
2020-02-12 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;
#------------------------------------------------------------------------------- 
# this cif originates from: 
#------------------------------------------------------------------------------- 
# leipzig university, faculty of chemistry and mineralogy, 
# johannisallee 29, 04103 leipzig, germany 
#------------------------------------------------------------------------------- 

#=============================================================================== 
#_leipzig_data_id data_x2878
#===============================================================================

_audit_creation_method           
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H14 Cl2 N3 O4 P W'
_chemical_formula_sum            'C20 H14 Cl2 N3 O4 P W'
_chemical_formula_weight         646.06

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'
W W -0.8490 6.8722 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5568(3)
_cell_length_b                   14.7613(5)
_cell_length_c                   15.4570(4)
_cell_angle_alpha                105.255(3)
_cell_angle_beta                 108.189(3)
_cell_angle_gamma                92.397(3)
_cell_volume                     2187.42(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    130.00(14)
_cell_measurement_reflns_used    15025
_cell_measurement_theta_min      2.3440
_cell_measurement_theta_max      32.2360

_exptl_crystal_description       needle
_exptl_crystal_colour            'clear intense red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.962
_exptl_crystal_F_000             1240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2500
_exptl_crystal_size_mid          0.0500
_exptl_crystal_size_min          0.0500
_exptl_absorpt_coefficient_mu    5.631
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.61046
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      130.00(14)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3560
_diffrn_reflns_number            35979
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.324
_diffrn_reflns_theta_max         32.533
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             14346
_reflns_number_gt                11210
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 4'
_computing_publication_material  SHELXL
_refine_special_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0169P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14346
_refine_ls_number_parameters     559
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0551
_refine_ls_wR_factor_gt          0.0504
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.21764(2) 0.25752(2) 0.47460(2) 0.01615(3) Uani 1 1 d . . . . .
W2 W 0.28102(2) 0.75815(2) 0.00728(2) 0.01706(3) Uani 1 1 d . . . . .
Cl1 Cl 0.60029(9) 0.50538(6) 0.62637(5) 0.03342(18) Uani 1 1 d . . . . .
Cl2 Cl 0.48769(10) 0.61767(6) 0.76439(7) 0.0412(2) Uani 1 1 d . . . . .
Cl3 Cl 0.41447(10) 1.11998(6) 0.25171(6) 0.0388(2) Uani 1 1 d . . . . .
Cl4 Cl 0.58918(9) 1.03684(6) 0.14639(7) 0.0379(2) Uani 1 1 d . . . . .
P1 P 0.11835(8) 0.11679(5) 0.59529(5) 0.01651(14) Uani 1 1 d . . . . .
P2 P 0.17710(8) 0.61466(5) 0.12476(5) 0.01865(15) Uani 1 1 d . . . . .
O1 O 0.1826(3) 0.47663(16) 0.50486(16) 0.0386(6) Uani 1 1 d . . . . .
O2 O 0.5085(2) 0.30812(15) 0.47531(14) 0.0264(5) Uani 1 1 d . . . . .
O3 O 0.2948(2) 0.04935(15) 0.42203(15) 0.0298(5) Uani 1 1 d . . . . .
O4 O 0.1219(2) 0.22670(15) 0.25492(13) 0.0267(5) Uani 1 1 d . . . . .
O5 O 0.2305(2) 0.97107(16) 0.01652(16) 0.0348(5) Uani 1 1 d . . . . .
O6 O 0.5790(2) 0.81404(16) 0.02544(15) 0.0283(5) Uani 1 1 d . . . . .
O7 O 0.3444(3) 0.54619(17) -0.04968(16) 0.0405(6) Uani 1 1 d . . . . .
O8 O 0.2091(2) 0.73101(16) -0.21102(14) 0.0303(5) Uani 1 1 d . . . . .
N1 N 0.2773(2) 0.28265(16) 0.63450(15) 0.0159(5) Uani 1 1 d . . . . .
N2 N -0.0227(3) 0.12766(17) 0.72206(16) 0.0202(5) Uani 1 1 d . . . . .
N3 N 0.0082(2) 0.22308(17) 0.47902(15) 0.0181(5) Uani 1 1 d . . . . .
N4 N 0.3339(2) 0.78268(16) 0.16690(15) 0.0176(5) Uani 1 1 d . . . . .
N5 N 0.0896(3) 0.47883(17) 0.18463(16) 0.0220(5) Uani 1 1 d . . . . .
N6 N 0.0704(2) 0.72383(16) 0.00877(15) 0.0182(5) Uani 1 1 d . . . . .
C1 C 0.2286(3) 0.22566(19) 0.67605(18) 0.0163(5) Uani 1 1 d . . . . .
C2 C 0.2706(3) 0.2457(2) 0.77507(19) 0.0207(6) Uani 1 1 d . . . . .
H2 H 0.2373 0.2058 0.8028 0.025 Uiso 1 1 calc R U . . .
C3 C 0.3619(3) 0.3251(2) 0.83131(19) 0.0220(6) Uani 1 1 d . . . . .
H3 H 0.3907 0.3391 0.8973 0.026 Uiso 1 1 calc R U . . .
C4 C 0.4101(3) 0.3836(2) 0.78862(19) 0.0213(6) Uani 1 1 d . . . . .
H4 H 0.4711 0.4378 0.8252 0.026 Uiso 1 1 calc R U . . .
C5 C 0.3660(3) 0.3601(2) 0.69129(19) 0.0208(6) Uani 1 1 d . . . . .
H5 H 0.3988 0.3995 0.6628 0.025 Uiso 1 1 calc R U . . .
C6 C 0.0550(3) 0.07623(19) 0.67898(18) 0.0174(5) Uani 1 1 d . . . . .
C7 C 0.0990(3) -0.0057(2) 0.69879(19) 0.0207(6) Uani 1 1 d . . . . .
H7 H 0.1530 -0.0390 0.6679 0.025 Uiso 1 1 calc R U . . .
C8 C 0.0613(3) -0.0373(2) 0.7653(2) 0.0239(6) Uani 1 1 d . . . . .
H8 H 0.0903 -0.0917 0.7803 0.029 Uiso 1 1 calc R U . . .
C9 C -0.0202(3) 0.0135(2) 0.8087(2) 0.0251(7) Uani 1 1 d . . . . .
H9 H -0.0479 -0.0063 0.8531 0.030 Uiso 1 1 calc R U . . .
C10 C -0.0598(3) 0.0945(2) 0.78512(19) 0.0232(6) Uani 1 1 d . . . . .
H10 H -0.1153 0.1280 0.8145 0.028 Uiso 1 1 calc R U . . .
C11 C -0.0234(3) 0.16699(19) 0.52920(18) 0.0168(5) Uani 1 1 d . . . . .
C12 C -0.1564(3) 0.1419(2) 0.52050(19) 0.0214(6) Uani 1 1 d . . . . .
H12 H -0.1762 0.1019 0.5534 0.026 Uiso 1 1 calc R U . . .
C13 C -0.2590(3) 0.1767(2) 0.4628(2) 0.0258(7) Uani 1 1 d . . . . .
H13 H -0.3482 0.1597 0.4559 0.031 Uiso 1 1 calc R U . . .
C14 C -0.2269(3) 0.2371(2) 0.4156(2) 0.0268(7) Uani 1 1 d . . . . .
H14 H -0.2939 0.2630 0.3782 0.032 Uiso 1 1 calc R U . . .
C15 C -0.0943(3) 0.2581(2) 0.42474(19) 0.0230(6) Uani 1 1 d . . . . .
H15 H -0.0737 0.2982 0.3922 0.028 Uiso 1 1 calc R U . . .
C16 C 0.1926(3) 0.3982(2) 0.4951(2) 0.0232(6) Uani 1 1 d . . . . .
C17 C 0.3995(3) 0.2906(2) 0.47565(18) 0.0201(6) Uani 1 1 d . . . . .
C18 C 0.2600(3) 0.1221(2) 0.44462(19) 0.0199(6) Uani 1 1 d . . . . .
C19 C 0.1560(3) 0.2384(2) 0.3373(2) 0.0206(6) Uani 1 1 d . . . . .
C20 C 0.2870(3) 0.72331(19) 0.20729(18) 0.0170(5) Uani 1 1 d . . . . .
C21 C 0.3339(3) 0.7401(2) 0.30627(19) 0.0214(6) Uani 1 1 d . . . . .
H21 H 0.3039 0.6979 0.3333 0.026 Uiso 1 1 calc R U . . .
C22 C 0.4244(3) 0.8190(2) 0.36307(19) 0.0230(6) Uani 1 1 d . . . . .
H22 H 0.4561 0.8306 0.4288 0.028 Uiso 1 1 calc R U . . .
C23 C 0.4678(3) 0.8809(2) 0.32187(19) 0.0230(6) Uani 1 1 d . . . . .
H23 H 0.5276 0.9354 0.3592 0.028 Uiso 1 1 calc R U . . .
C24 C 0.4206(3) 0.8602(2) 0.22463(19) 0.0206(6) Uani 1 1 d . . . . .
H24 H 0.4501 0.9020 0.1971 0.025 Uiso 1 1 calc R U . . .
C25 C 0.0961(3) 0.5732(2) 0.20013(18) 0.0176(6) Uani 1 1 d . . . . .
C26 C 0.0413(3) 0.6312(2) 0.26261(19) 0.0213(6) Uani 1 1 d . . . . .
H26 H 0.0470 0.6962 0.2711 0.026 Uiso 1 1 calc R U . . .
C27 C -0.0214(3) 0.5895(2) 0.31122(19) 0.0222(6) Uani 1 1 d . . . . .
H27 H -0.0569 0.6264 0.3544 0.027 Uiso 1 1 calc R U . . .
C28 C -0.0309(3) 0.4925(2) 0.2953(2) 0.0239(6) Uani 1 1 d . . . . .
H28 H -0.0748 0.4630 0.3263 0.029 Uiso 1 1 calc R U . . .
C29 C 0.0259(3) 0.4402(2) 0.2325(2) 0.0243(6) Uani 1 1 d . . . . .
H29 H 0.0200 0.3750 0.2227 0.029 Uiso 1 1 calc R U . . .
C30 C 0.0377(3) 0.6660(2) 0.05635(18) 0.0181(6) Uani 1 1 d . . . . .
C31 C -0.0962(3) 0.6409(2) 0.04606(19) 0.0238(6) Uani 1 1 d . . . . .
H31 H -0.1174 0.5987 0.0764 0.029 Uiso 1 1 calc R U . . .
C32 C -0.1971(3) 0.6786(2) -0.0092(2) 0.0277(7) Uani 1 1 d . . . . .
H32 H -0.2866 0.6615 -0.0170 0.033 Uiso 1 1 calc R U . . .
C33 C -0.1633(3) 0.7419(2) -0.0527(2) 0.0271(7) Uani 1 1 d . . . . .
H33 H -0.2290 0.7706 -0.0877 0.032 Uiso 1 1 calc R U . . .
C34 C -0.0304(3) 0.7615(2) -0.04305(19) 0.0230(6) Uani 1 1 d . . . . .
H34 H -0.0084 0.8030 -0.0738 0.028 Uiso 1 1 calc R U . . .
C35 C 0.2500(3) 0.8956(2) 0.01819(19) 0.0214(6) Uani 1 1 d . . . . .
C36 C 0.4673(3) 0.7936(2) 0.01835(19) 0.0205(6) Uani 1 1 d . . . . .
C37 C 0.3173(3) 0.6206(2) -0.0240(2) 0.0230(6) Uani 1 1 d . . . . .
C38 C 0.2337(3) 0.7405(2) -0.1297(2) 0.0217(6) Uani 1 1 d . . . . .
C39 C 0.6248(4) 0.6089(2) 0.7208(2) 0.0320(8) Uani 1 1 d . . . . .
H39A H 0.6369 0.6637 0.6993 0.038 Uiso 1 1 calc R U . . .
H39B H 0.7063 0.6093 0.7722 0.038 Uiso 1 1 calc R U . . .
C40 C 0.4908(4) 1.1273(2) 0.1662(2) 0.0344(8) Uani 1 1 d . . . . .
H40A H 0.4212 1.1240 0.1067 0.041 Uiso 1 1 calc R U . . .
H40B H 0.5468 1.1881 0.1878 0.041 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C19 1.952(3) . ?
W1 C17 1.955(3) . ?
W1 C18 2.032(3) . ?
W1 C16 2.057(3) . ?
W1 N1 2.274(2) . ?
W1 N3 2.274(2) . ?
W2 C36 1.957(3) . ?
W2 C38 1.960(3) . ?
W2 C35 2.041(3) . ?
W2 C37 2.041(3) . ?
W2 N6 2.268(2) . ?
W2 N4 2.277(2) . ?
Cl1 C39 1.758(3) . ?
Cl2 C39 1.773(3) . ?
Cl3 C40 1.772(3) . ?
Cl4 C40 1.748(3) . ?
P1 C11 1.835(3) . ?
P1 C1 1.837(3) . ?
P1 C6 1.842(3) . ?
P2 C20 1.841(3) . ?
P2 C30 1.845(3) . ?
P2 C25 1.848(3) . ?
O1 C16 1.142(4) . ?
O2 C17 1.170(3) . ?
O3 C18 1.151(3) . ?
O4 C19 1.173(3) . ?
O5 C35 1.146(4) . ?
O6 C36 1.169(3) . ?
O7 C37 1.146(4) . ?
O8 C38 1.169(3) . ?
N1 C5 1.351(3) . ?
N1 C1 1.356(3) . ?
N2 C10 1.348(3) . ?
N2 C6 1.349(3) . ?
N3 C15 1.360(4) . ?
N3 C11 1.369(3) . ?
N4 C24 1.345(3) . ?
N4 C20 1.360(3) . ?
N5 C25 1.345(4) . ?
N5 C29 1.352(4) . ?
N6 C34 1.355(4) . ?
N6 C30 1.361(3) . ?
C1 C2 1.398(4) . ?
C2 C3 1.379(4) . ?
C3 C4 1.384(4) . ?
C4 C5 1.369(4) . ?
C6 C7 1.388(4) . ?
C7 C8 1.388(4) . ?
C8 C9 1.379(4) . ?
C9 C10 1.384(4) . ?
C11 C12 1.393(4) . ?
C12 C13 1.384(4) . ?
C13 C14 1.384(4) . ?
C14 C15 1.375(4) . ?
C20 C21 1.402(4) . ?
C21 C22 1.373(4) . ?
C22 C23 1.380(4) . ?
C23 C24 1.371(4) . ?
C25 C26 1.398(4) . ?
C26 C27 1.378(4) . ?
C27 C28 1.381(4) . ?
C28 C29 1.380(4) . ?
C30 C31 1.395(4) . ?
C31 C32 1.380(4) . ?
C32 C33 1.380(4) . ?
C33 C34 1.374(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
C19 W1 C17 87.56(11) . . ?
C19 W1 C18 86.25(11) . . ?
C17 W1 C18 84.69(12) . . ?
C19 W1 C16 89.45(12) . . ?
C17 W1 C16 88.39(12) . . ?
C18 W1 C16 172.00(11) . . ?
C19 W1 N1 176.55(10) . . ?
C17 W1 N1 95.38(10) . . ?
C18 W1 N1 95.82(9) . . ?
C16 W1 N1 88.81(10) . . ?
C19 W1 N3 94.28(10) . . ?
C17 W1 N3 177.80(9) . . ?
C18 W1 N3 96.63(10) . . ?
C16 W1 N3 90.41(10) . . ?
N1 W1 N3 82.75(8) . . ?
C36 W2 C38 87.30(12) . . ?
C36 W2 C35 88.78(12) . . ?
C38 W2 C35 86.14(11) . . ?
C36 W2 C37 87.11(12) . . ?
C38 W2 C37 85.20(12) . . ?
C35 W2 C37 170.57(11) . . ?
C36 W2 N6 174.81(9) . . ?
C38 W2 N6 97.59(10) . . ?
C35 W2 N6 89.81(10) . . ?
C37 W2 N6 95.02(10) . . ?
C36 W2 N4 93.00(10) . . ?
C38 W2 N4 178.39(11) . . ?
C35 W2 N4 92.28(9) . . ?
C37 W2 N4 96.40(10) . . ?
N6 W2 N4 82.07(8) . . ?
C11 P1 C1 100.56(13) . . ?
C11 P1 C6 103.76(13) . . ?
C1 P1 C6 100.40(12) . . ?
C20 P2 C30 100.46(13) . . ?
C20 P2 C25 103.03(12) . . ?
C30 P2 C25 100.10(13) . . ?
C5 N1 C1 118.3(2) . . ?
C5 N1 W1 117.41(17) . . ?
C1 N1 W1 124.28(18) . . ?
C10 N2 C6 116.7(3) . . ?
C15 N3 C11 117.6(2) . . ?
C15 N3 W1 117.32(18) . . ?
C11 N3 W1 125.05(19) . . ?
C24 N4 C20 118.2(2) . . ?
C24 N4 W2 117.17(17) . . ?
C20 N4 W2 124.58(18) . . ?
C25 N5 C29 116.9(2) . . ?
C34 N6 C30 117.7(3) . . ?
C34 N6 W2 117.87(19) . . ?
C30 N6 W2 124.46(19) . . ?
N1 C1 C2 120.9(3) . . ?
N1 C1 P1 116.23(18) . . ?
C2 C1 P1 122.6(2) . . ?
C3 C2 C1 119.5(3) . . ?
C2 C3 C4 119.4(2) . . ?
C5 C4 C3 118.5(3) . . ?
N1 C5 C4 123.4(3) . . ?
N2 C6 C7 123.0(2) . . ?
N2 C6 P1 120.8(2) . . ?
C7 C6 P1 116.1(2) . . ?
C6 C7 C8 119.1(3) . . ?
C9 C8 C7 118.6(3) . . ?
C8 C9 C10 118.8(3) . . ?
N2 C10 C9 123.8(3) . . ?
N3 C11 C12 121.2(3) . . ?
N3 C11 P1 115.1(2) . . ?
C12 C11 P1 123.2(2) . . ?
C13 C12 C11 119.8(3) . . ?
C14 C13 C12 119.1(3) . . ?
C15 C14 C13 118.9(3) . . ?
N3 C15 C14 123.2(3) . . ?
O1 C16 W1 177.2(3) . . ?
O2 C17 W1 178.3(3) . . ?
O3 C18 W1 171.0(2) . . ?
O4 C19 W1 178.5(3) . . ?
N4 C20 C21 120.5(3) . . ?
N4 C20 P2 116.23(18) . . ?
C21 C20 P2 122.8(2) . . ?
C22 C21 C20 119.7(3) . . ?
C21 C22 C23 119.5(3) . . ?
C24 C23 C22 118.4(3) . . ?
N4 C24 C23 123.6(3) . . ?
N5 C25 C26 123.2(2) . . ?
N5 C25 P2 111.95(19) . . ?
C26 C25 P2 124.8(2) . . ?
C27 C26 C25 118.3(3) . . ?
C26 C27 C28 119.4(3) . . ?
C29 C28 C27 118.8(3) . . ?
N5 C29 C28 123.3(3) . . ?
N6 C30 C31 120.9(3) . . ?
N6 C30 P2 116.5(2) . . ?
C31 C30 P2 122.4(2) . . ?
C32 C31 C30 120.0(3) . . ?
C31 C32 C33 119.1(3) . . ?
C34 C33 C32 118.5(3) . . ?
N6 C34 C33 123.6(3) . . ?
O5 C35 W2 174.4(2) . . ?
O6 C36 W2 179.3(3) . . ?
O7 C37 W2 171.2(2) . . ?
O8 C38 W2 178.1(3) . . ?
Cl1 C39 Cl2 112.30(18) . . ?
Cl4 C40 Cl3 112.58(18) . . ?

_refine_diff_density_max         1.847
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.141

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_I_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1983663'
_audit_update_record             
;
2020-02-12 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   9.3290(3)
_cell_length_b                   14.1222(5)
_cell_length_c                   14.9039(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.6570(13)
_cell_angle_gamma                90
_cell_volume                     1961.42(12)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mo -0.0483 2.7339 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584
4.3875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C21 H18 Mo1 N3 O3 P1 
# Dc =      1.65 Fooo =    984.00 Mu =     64.87 M =    487.31
# Found Formula = C21 H18 Mo1 N3 O3 P1 
# Dc =      1.65 FOOO =    984.00 Mu =     64.87 M =    487.31

_chemical_formula_sum            'C21 H18 Mo1 N3 O3 P1'
_chemical_formula_moiety         'C21 H18 Mo1 N3 O3 P1'
_chemical_compound_source        synthetic
_chemical_formula_weight         487.31


_cell_measurement_reflns_used    9931
_cell_measurement_theta_min      4
_cell_measurement_theta_max      67
_cell_measurement_temperature    180

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.060
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.210

_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             984
_exptl_absorpt_coefficient_mu    6.487

# Sheldrick geometric approximatio 0.38 0.68 
# No experimental values of Tmin/max available 
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.5041
_exptl_absorpt_correction_T_max  0.7528
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_measurement_method       ω/2θ

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      180
_diffrn_reflns_number            18321
_reflns_number_total             3484
_diffrn_reflns_av_R_equivalents  0.038
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 3484 
# Theoretical number of reflections is about 6972 


_diffrn_reflns_theta_min         4.315
_diffrn_reflns_theta_max         66.861
_diffrn_measured_fraction_theta_max 0.997

_diffrn_reflns_theta_full        66.861
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_reflns_limit_h_min              -11
_reflns_limit_h_max              11
_reflns_limit_k_min              0
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              17

_oxford_diffrn_Wilson_B_factor   1.36
_oxford_diffrn_Wilson_scale      6.22

_atom_sites_solution_primary     other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.48
_refine_diff_density_max         0.41


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_restraints     0
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3468
_oxford_refine_ls_R_factor_ref   0.0259
_refine_ls_wR_factor_ref         0.0593
_refine_ls_goodness_of_fit_ref   0.9420
_refine_ls_shift/su_max          0.0013769
_refine_ls_shift/su_mean         0.0000736


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        3468
_refine_ls_R_factor_all          0.0259
_refine_ls_wR_factor_all         0.0593

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3207
_refine_ls_R_factor_gt           0.0231
_refine_ls_wR_factor_gt          0.0559


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 36.2 58.6 34.9 15.0 3.81 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mo1 Mo 0.465724(17) 0.289895(12) 0.702889(11) 0.0167 1.0000 Uani . . . . . .
P1 P 0.12611(6) 0.24450(4) 0.78931(4) 0.0210 1.0000 Uani . . . . . .
N1 N 0.3442(2) 0.38082(13) 0.81017(12) 0.0205 1.0000 Uani . . . . . .
N2 N 0.2456(2) 0.27354(13) 0.62101(12) 0.0180 1.0000 Uani . . . . . .
N3 N 0.3995(2) 0.15695(13) 0.78419(12) 0.0200 1.0000 Uani . . . . . .
O1 O 0.6470(2) 0.18443(18) 0.56547(14) 0.0475 1.0000 Uani . . . . . .
O2 O 0.77399(18) 0.31851(15) 0.78420(13) 0.0363 1.0000 Uani . . . . . .
O3 O 0.5843(2) 0.46168(15) 0.59968(14) 0.0449 1.0000 Uani . . . . . .
C1 C 0.2057(2) 0.35759(16) 0.82495(14) 0.0201 1.0000 Uani . . . . . .
C2 C 0.1144(3) 0.41463(18) 0.87220(16) 0.0285 1.0000 Uani . . . . . .
C3 C 0.1653(3) 0.49803(19) 0.90913(19) 0.0356 1.0000 Uani . . . . . .
C4 C 0.3073(3) 0.51940(18) 0.89949(18) 0.0335 1.0000 Uani . . . . . .
C5 C 0.3952(3) 0.46113(17) 0.85014(16) 0.0266 1.0000 Uani . . . . . .
C6 C 0.5485(3) 0.4886(2) 0.8423(2) 0.0470 1.0000 Uani . . . . . .
C7 C 0.1265(2) 0.25378(16) 0.66686(15) 0.0192 1.0000 Uani . . . . . .
C8 C -0.0084(3) 0.24138(18) 0.62519(17) 0.0251 1.0000 Uani . . . . . .
C9 C -0.0244(3) 0.24575(19) 0.53274(17) 0.0280 1.0000 Uani . . . . . .
C10 C 0.0959(3) 0.26440(18) 0.48570(16) 0.0250 1.0000 Uani . . . . . .
C11 C 0.2289(3) 0.27936(16) 0.53008(16) 0.0214 1.0000 Uani . . . . . .
C12 C 0.3533(3) 0.3037(2) 0.47429(17) 0.0316 1.0000 Uani . . . . . .
C13 C 0.2671(2) 0.15876(16) 0.81990(14) 0.0204 1.0000 Uani . . . . . .
C14 C 0.2246(3) 0.09364(18) 0.88221(17) 0.0317 1.0000 Uani . . . . . .
C15 C 0.3171(4) 0.0222(2) 0.9101(2) 0.0429 1.0000 Uani . . . . . .
C16 C 0.4466(3) 0.01648(18) 0.87074(19) 0.0371 1.0000 Uani . . . . . .
C17 C 0.4866(3) 0.08364(17) 0.80836(17) 0.0269 1.0000 Uani . . . . . .
C18 C 0.6289(3) 0.0726(2) 0.7670(2) 0.0383 1.0000 Uani . . . . . .
C19 C 0.5727(3) 0.22130(19) 0.61620(18) 0.0290 1.0000 Uani . . . . . .
C20 C 0.6544(3) 0.30510(17) 0.75954(16) 0.0237 1.0000 Uani . . . . . .
C21 C 0.5306(3) 0.40006(19) 0.63816(17) 0.0277 1.0000 Uani . . . . . .
H21 H 0.0211 0.3956 0.8783 0.0341 1.0000 Uiso R . . . . .
H31 H 0.1051 0.5379 0.9387 0.0426 1.0000 Uiso R . . . . .
H41 H 0.3467 0.5742 0.9265 0.0417 1.0000 Uiso R . . . . .
H61 H 0.6096 0.4362 0.8595 0.0717 1.0000 Uiso R . . . . .
H62 H 0.5693 0.5432 0.8792 0.0715 1.0000 Uiso R . . . . .
H63 H 0.5658 0.5045 0.7813 0.0717 1.0000 Uiso R . . . . .
H81 H -0.0842 0.2306 0.6615 0.0301 1.0000 Uiso R . . . . .
H91 H -0.1138 0.2367 0.5029 0.0342 1.0000 Uiso R . . . . .
H101 H 0.0869 0.2680 0.4244 0.0306 1.0000 Uiso R . . . . .
H121 H 0.3969 0.3627 0.4941 0.0481 1.0000 Uiso R . . . . .
H122 H 0.3212 0.3112 0.4116 0.0481 1.0000 Uiso R . . . . .
H123 H 0.4259 0.2553 0.4783 0.0481 1.0000 Uiso R . . . . .
H141 H 0.1352 0.0988 0.9048 0.0387 1.0000 Uiso R . . . . .
H151 H 0.2922 -0.0207 0.9543 0.0522 1.0000 Uiso R . . . . .
H161 H 0.5088 -0.0322 0.8863 0.0442 1.0000 Uiso R . . . . .
H181 H 0.6856 0.1273 0.7780 0.0569 1.0000 Uiso R . . . . .
H182 H 0.6731 0.0186 0.7919 0.0575 1.0000 Uiso R . . . . .
H183 H 0.6155 0.0643 0.7028 0.0566 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.4073(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mo1 . N1 . 2.3790(18) yes
Mo1 . N2 . 2.3508(18) yes
Mo1 . N3 . 2.3332(19) yes
Mo1 . C19 . 1.929(3) yes
Mo1 . C20 . 1.929(2) yes
Mo1 . C21 . 1.942(3) yes
P1 . C1 . 1.830(2) yes
P1 . C7 . 1.830(2) yes
P1 . C13 . 1.830(2) yes
N1 . C1 . 1.361(3) yes
N1 . C5 . 1.357(3) yes
N2 . C7 . 1.360(3) yes
N2 . C11 . 1.359(3) yes
N3 . C13 . 1.368(3) yes
N3 . C17 . 1.354(3) yes
O1 . C19 . 1.171(3) yes
O2 . C20 . 1.174(3) yes
O3 . C21 . 1.168(3) yes
C1 . C2 . 1.388(3) yes
C2 . C3 . 1.375(4) yes
C2 . H21 . 0.920 no
C3 . C4 . 1.373(4) yes
C3 . H31 . 0.921 no
C4 . C5 . 1.395(4) yes
C4 . H41 . 0.940 no
C5 . C6 . 1.491(4) yes
C6 . H61 . 0.962 no
C6 . H62 . 0.962 no
C6 . H63 . 0.957 no
C7 . C8 . 1.388(3) yes
C8 . C9 . 1.380(4) yes
C8 . H81 . 0.923 no
C9 . C10 . 1.377(4) yes
C9 . H91 . 0.935 no
C10 . C11 . 1.395(3) yes
C10 . H101 . 0.915 no
C11 . C12 . 1.498(3) yes
C12 . H121 . 0.967 no
C12 . H122 . 0.973 no
C12 . H123 . 0.963 no
C13 . C14 . 1.378(3) yes
C14 . C15 . 1.380(4) yes
C14 . H141 . 0.916 no
C15 . C16 . 1.370(4) yes
C15 . H151 . 0.932 no
C16 . C17 . 1.391(4) yes
C16 . H161 . 0.922 no
C17 . C18 . 1.497(4) yes
C18 . H181 . 0.947 no
C18 . H182 . 0.936 no
C18 . H183 . 0.967 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Mo1 . N2 . 88.27(6) yes
N1 . Mo1 . N3 . 86.53(6) yes
N2 . Mo1 . N3 . 86.83(6) yes
N1 . Mo1 . C19 . 176.84(9) yes
N2 . Mo1 . C19 . 93.98(9) yes
N3 . Mo1 . C19 . 95.81(9) yes
N1 . Mo1 . C20 . 95.71(8) yes
N2 . Mo1 . C20 . 174.68(8) yes
N3 . Mo1 . C20 . 96.91(8) yes
C19 . Mo1 . C20 . 81.91(10) yes
N1 . Mo1 . C21 . 94.06(9) yes
N2 . Mo1 . C21 . 96.07(8) yes
N3 . Mo1 . C21 . 177.06(8) yes
C19 . Mo1 . C21 . 83.50(11) yes
C20 . Mo1 . C21 . 80.16(10) yes
C1 . P1 . C7 . 101.97(10) yes
C1 . P1 . C13 . 103.17(10) yes
C7 . P1 . C13 . 105.13(10) yes
Mo1 . N1 . C1 . 117.67(15) yes
Mo1 . N1 . C5 . 125.29(16) yes
C1 . N1 . C5 . 116.5(2) yes
Mo1 . N2 . C7 . 118.27(14) yes
Mo1 . N2 . C11 . 124.64(15) yes
C7 . N2 . C11 . 117.05(19) yes
Mo1 . N3 . C13 . 116.91(14) yes
Mo1 . N3 . C17 . 125.69(16) yes
C13 . N3 . C17 . 116.9(2) yes
P1 . C1 . N1 . 122.62(17) yes
P1 . C1 . C2 . 113.81(18) yes
N1 . C1 . C2 . 123.5(2) yes
C1 . C2 . C3 . 119.5(2) yes
C1 . C2 . H21 . 119.1 no
C3 . C2 . H21 . 121.4 no
C2 . C3 . C4 . 117.6(2) yes
C2 . C3 . H31 . 120.5 no
C4 . C3 . H31 . 121.9 no
C3 . C4 . C5 . 121.3(2) yes
C3 . C4 . H41 . 119.8 no
C5 . C4 . H41 . 118.9 no
C4 . C5 . N1 . 121.4(2) yes
C4 . C5 . C6 . 118.5(2) yes
N1 . C5 . C6 . 120.1(2) yes
C5 . C6 . H61 . 109.8 no
C5 . C6 . H62 . 109.4 no
H61 . C6 . H62 . 111.3 no
C5 . C6 . H63 . 109.9 no
H61 . C6 . H63 . 108.0 no
H62 . C6 . H63 . 108.4 no
P1 . C7 . N2 . 123.73(16) yes
P1 . C7 . C8 . 113.16(17) yes
N2 . C7 . C8 . 123.1(2) yes
C7 . C8 . C9 . 119.7(2) yes
C7 . C8 . H81 . 117.5 no
C9 . C8 . H81 . 122.8 no
C8 . C9 . C10 . 117.6(2) yes
C8 . C9 . H91 . 121.4 no
C10 . C9 . H91 . 121.0 no
C9 . C10 . C11 . 121.1(2) yes
C9 . C10 . H101 . 118.6 no
C11 . C10 . H101 . 120.3 no
C10 . C11 . N2 . 121.5(2) yes
C10 . C11 . C12 . 117.8(2) yes
N2 . C11 . C12 . 120.8(2) yes
C11 . C12 . H121 . 110.7 no
C11 . C12 . H122 . 110.2 no
H121 . C12 . H122 . 107.8 no
C11 . C12 . H123 . 111.3 no
H121 . C12 . H123 . 108.0 no
H122 . C12 . H123 . 108.7 no
P1 . C13 . N3 . 124.56(17) yes
P1 . C13 . C14 . 112.53(19) yes
N3 . C13 . C14 . 122.9(2) yes
C13 . C14 . C15 . 119.7(3) yes
C13 . C14 . H141 . 119.4 no
C15 . C14 . H141 . 120.9 no
C14 . C15 . C16 . 117.8(3) yes
C14 . C15 . H151 . 121.0 no
C16 . C15 . H151 . 121.2 no
C15 . C16 . C17 . 121.0(3) yes
C15 . C16 . H161 . 119.6 no
C17 . C16 . H161 . 119.4 no
C16 . C17 . N3 . 121.5(2) yes
C16 . C17 . C18 . 118.3(2) yes
N3 . C17 . C18 . 120.2(2) yes
C17 . C18 . H181 . 110.1 no
C17 . C18 . H182 . 107.8 no
H181 . C18 . H182 . 111.4 no
C17 . C18 . H183 . 110.1 no
H181 . C18 . H183 . 108.4 no
H182 . C18 . H183 . 109.1 no
O1 . C19 . Mo1 . 174.5(2) yes
O2 . C20 . Mo1 . 171.9(2) yes
O3 . C21 . Mo1 . 172.6(2) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C6 . H61 . O2 . 138 0.96 2.56 3.334(4) yes
C6 . H61 . C20 . 123 0.96 2.42 3.054(4) yes
C9 . H91 . O1 1_455 130 0.94 2.57 3.244(4) yes
C12 . H121 . C21 . 129 0.97 2.49 3.190(4) yes
C12 . H123 . O1 . 148 0.96 2.59 3.442(4) yes
C12 . H123 . C19 . 123 0.96 2.46 3.101(4) yes
C18 . H181 . C20 . 137 0.95 2.54 3.295(4) yes


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_added_by_encifer_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1983666'
_audit_update_record             
;
2020-02-12 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;
#------------------------------------------------------------------------------- 
# this cif originates from: 
#------------------------------------------------------------------------------- 
# leipzig university, faculty of chemistry and mineralogy, 
# johannisallee 29, 04103 leipzig, germany 
#------------------------------------------------------------------------------- 

#=============================================================================== 
#_leipzig_data_id data_x2874
#===============================================================================

_audit_creation_method           
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H18 Br6 Mo N6 O4 P2'
_chemical_formula_sum            'C34 H18 Br6 Mo N6 O4 P2'
_chemical_formula_weight         1211.88

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7277(6)
_cell_length_b                   11.7959(5)
_cell_length_c                   19.1179(7)
_cell_angle_alpha                79.702(3)
_cell_angle_beta                 84.994(4)
_cell_angle_gamma                65.607(5)
_cell_volume                     2167.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    130.00(14)
_cell_measurement_reflns_used    7122
_cell_measurement_theta_min      2.5770
_cell_measurement_theta_max      30.7460

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_F_000             1156
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.1000
_exptl_absorpt_coefficient_mu    5.949
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.78859
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130.00(14)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3560
_diffrn_reflns_number            27582
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.288
_diffrn_reflns_theta_max         32.405
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             14088
_reflns_number_gt                9517
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 4'
_computing_publication_material  SHELXL

_refine_special_details          
;
The unit cell contains two heavily disordered hexane molecules, which 
have been treated as a diffuse contribution to the overall scattering 
without specific atom positions by squeeze/Platon. The solvent 
assessible void was found to be in the position (ï?1/20.004, 0.000, 0.500) 
with a volume of 332.3 ï?1/23 and 103.2 electrons. The calculated number of 
electrons matches with the electron count of two n-hexane molecules. 
A disordered N-C-Br unit within one ligand was refined over two positions. 
All of the non-H atoms were refined anisotropically, but with the 
application of ISOR restraints in the case of the disordered pyridyl moiety. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0437P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14088
_refine_ls_number_parameters     506
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0449
_refine_ls_wR_factor_ref         0.1064
_refine_ls_wR_factor_gt          0.0961
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.34930(3) 0.74204(3) 0.23432(2) 0.02097(7) Uani 1 1 d . . . . .
Br1 Br 0.79931(4) 0.60361(4) 0.03204(2) 0.03880(10) Uani 1 1 d . . . . .
Br2 Br 0.65673(6) 0.74264(5) 0.47371(2) 0.05718(14) Uani 1 1 d . . . . .
Br5 Br 0.27357(4) 1.03874(3) -0.03032(2) 0.02846(8) Uani 1 1 d . . . . .
Br6 Br 0.28306(4) 0.17900(4) 0.14992(2) 0.03644(10) Uani 1 1 d . . . . .
Br7 Br 0.00681(4) 0.49309(5) 0.39212(2) 0.04683(12) Uani 1 1 d . . . . .
P1 P 0.53646(9) 0.52939(8) 0.27761(4) 0.02136(17) Uani 1 1 d . . . . .
P2 P 0.23616(8) 0.65949(8) 0.15997(4) 0.01821(16) Uani 1 1 d . . . . .
O1 O 0.1589(3) 0.7296(3) 0.36867(13) 0.0412(7) Uani 1 1 d . . . . .
O2 O 0.1124(3) 1.0068(3) 0.18710(14) 0.0356(6) Uani 1 1 d . . . . .
O3 O 0.5168(3) 0.8247(3) 0.10416(15) 0.0422(7) Uani 1 1 d . . . . .
O4 O 0.4636(4) 0.8876(3) 0.3145(2) 0.0800(14) Uani 1 1 d . . . . .
N1 N 0.6965(3) 0.5426(3) 0.16276(14) 0.0235(6) Uani 1 1 d . . . . .
N2 N 0.6033(3) 0.6074(3) 0.38714(14) 0.0261(6) Uani 1 1 d . . . . .
N5 N 0.2296(3) 0.8454(3) 0.05398(13) 0.0207(5) Uani 1 1 d . . . . .
N6 N 0.2772(3) 0.4157(3) 0.14778(13) 0.0216(5) Uani 1 1 d . . . . .
N7 N 0.0894(3) 0.5891(3) 0.26422(14) 0.0270(6) Uani 1 1 d . . . . .
C1 C 0.7036(3) 0.4847(3) 0.23081(16) 0.0233(7) Uani 1 1 d . . . . .
C2 C 0.8266(4) 0.4013(4) 0.26170(18) 0.0333(8) Uani 1 1 d . . . . .
H2 H 0.8288 0.3609 0.3083 0.040 Uiso 1 1 calc R U . . .
C3 C 0.9447(4) 0.3793(4) 0.2226(2) 0.0383(9) Uani 1 1 d . . . . .
H3 H 1.0283 0.3240 0.2427 0.046 Uiso 1 1 calc R U . . .
C4 C 0.9406(4) 0.4387(4) 0.15322(19) 0.0320(8) Uani 1 1 d . . . . .
H4 H 1.0198 0.4260 0.1257 0.038 Uiso 1 1 calc R U . . .
C5 C 0.8133(3) 0.5176(3) 0.12699(16) 0.0243(7) Uani 1 1 d . . . . .
C6 C 0.5940(3) 0.5053(3) 0.36982(16) 0.0234(7) Uani 1 1 d . . . . .
C7 C 0.6278(4) 0.3937(4) 0.41663(18) 0.0316(8) Uani 1 1 d . . . . .
H7 H 0.6190 0.3248 0.4040 0.038 Uiso 1 1 calc R U . . .
C8 C 0.6759(4) 0.3870(4) 0.48410(19) 0.0378(9) Uani 1 1 d . . . . .
H8 H 0.6997 0.3130 0.5167 0.045 Uiso 1 1 calc R U . . .
C9 C 0.6874(4) 0.4888(4) 0.50128(18) 0.0345(9) Uani 1 1 d . . . . .
H9 H 0.7214 0.4863 0.5449 0.041 Uiso 1 1 calc R U . . .
C10 C 0.6467(4) 0.5957(4) 0.45126(19) 0.0319(8) Uani 1 1 d . . . . .
C11 C 0.5081(4) 0.3834(3) 0.28456(17) 0.0262(7) Uani 1 1 d . . . . .
C12 C 0.3861(4) 0.3820(4) 0.31256(18) 0.0316(8) Uani 1 1 d . . . . .
H12 H 0.3147 0.4553 0.3234 0.038 Uiso 1 1 calc R U . . .
C13 C 0.3727(5) 0.2689(4) 0.3240(2) 0.0441(11) Uani 1 1 d . . . . .
H13 H 0.2910 0.2649 0.3421 0.053 Uiso 1 1 calc R U . . .
C14 C 0.4796(6) 0.1633(5) 0.3088(2) 0.0566(14) Uani 1 1 d . . . . .
H14 H 0.4686 0.0885 0.3115 0.068 Uiso 1 1 calc R U . A 1
C17 C 0.1866(3) 0.7518(3) 0.07018(15) 0.0192(6) Uani 1 1 d . . . . .
C18 C 0.1151(3) 0.7262(3) 0.02288(16) 0.0227(6) Uani 1 1 d . . . . .
H18 H 0.0894 0.6588 0.0349 0.027 Uiso 1 1 calc R U . . .
C19 C 0.0821(3) 0.8029(3) -0.04304(17) 0.0256(7) Uani 1 1 d . . . . .
H19 H 0.0307 0.7897 -0.0750 0.031 Uiso 1 1 calc R U . . .
C20 C 0.1266(3) 0.8982(3) -0.06010(17) 0.0276(7) Uani 1 1 d . . . . .
H20 H 0.1071 0.9506 -0.1039 0.033 Uiso 1 1 calc R U . . .
C21 C 0.2011(3) 0.9135(3) -0.01016(17) 0.0226(6) Uani 1 1 d . . . . .
C22 C 0.3292(3) 0.5027(3) 0.13387(15) 0.0200(6) Uani 1 1 d . . . . .
C23 C 0.4571(3) 0.4809(3) 0.10110(17) 0.0260(7) Uani 1 1 d . . . . .
H23 H 0.4900 0.5438 0.0923 0.031 Uiso 1 1 calc R U . . .
C24 C 0.5335(4) 0.3634(4) 0.0822(2) 0.0332(8) Uani 1 1 d . . . . .
H24 H 0.6182 0.3466 0.0597 0.040 Uiso 1 1 calc R U . . .
C25 C 0.4829(4) 0.2710(4) 0.0970(2) 0.0351(8) Uani 1 1 d . . . . .
H25 H 0.5327 0.1905 0.0860 0.042 Uiso 1 1 calc R U . . .
C26 C 0.3547(3) 0.3042(3) 0.12914(18) 0.0263(7) Uani 1 1 d . . . . .
C27 C 0.0740(3) 0.6593(3) 0.19929(16) 0.0217(6) Uani 1 1 d . . . . .
C28 C -0.0538(3) 0.7366(3) 0.17192(17) 0.0232(7) Uani 1 1 d . . . . .
H28 H -0.0625 0.7837 0.1267 0.028 Uiso 1 1 calc R U . . .
C29 C -0.1697(3) 0.7429(3) 0.21336(17) 0.0258(7) Uani 1 1 d . . . . .
H29 H -0.2566 0.7946 0.1959 0.031 Uiso 1 1 calc R U . . .
C30 C -0.1551(4) 0.6729(4) 0.27966(18) 0.0283(7) Uani 1 1 d . . . . .
H30 H -0.2302 0.6764 0.3089 0.034 Uiso 1 1 calc R U . . .
C31 C -0.0216(4) 0.5959(4) 0.30109(17) 0.0290(8) Uani 1 1 d . . . . .
C32 C 0.2311(4) 0.7258(3) 0.31978(17) 0.0279(7) Uani 1 1 d . . . . .
C33 C 0.2002(4) 0.9094(3) 0.20318(18) 0.0283(7) Uani 1 1 d . . . . .
C34 C 0.4620(4) 0.7855(4) 0.1484(2) 0.0307(8) Uani 1 1 d . . . . .
C35 C 0.4257(4) 0.8288(4) 0.2873(2) 0.0414(10) Uani 1 1 d . . . . .
Br3 Br 0.7723(9) 0.0260(7) 0.2679(5) 0.1093(17) Uani 0.40(2) 1 d . U P B 1
N3 N 0.6333(13) 0.2742(11) 0.2752(6) 0.026(2) Uani 0.40(2) 1 d . U P B 1
C15 C 0.6222(14) 0.1680(11) 0.2865(6) 0.025(3) Uani 0.40(2) 1 d . U P B 1
Br4 Br 0.7316(13) 0.0365(5) 0.2471(6) 0.124(2) Uani 0.60(2) 1 d . U P B 2
N4 N 0.6019(10) 0.2853(8) 0.2624(5) 0.0327(19) Uani 0.60(2) 1 d . U P B 2
C16 C 0.5787(13) 0.1800(8) 0.2748(5) 0.039(2) Uani 0.60(2) 1 d . U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C33 1.987(4) . ?
Mo1 C35 1.989(3) . ?
Mo1 C32 2.010(4) . ?
Mo1 C34 2.071(4) . ?
Mo1 P2 2.4928(8) . ?
Mo1 P1 2.5290(10) . ?
Br1 C5 1.900(3) . ?
Br2 C10 1.904(4) . ?
Br5 C21 1.905(3) . ?
Br6 C26 1.899(3) . ?
Br7 C31 1.904(3) . ?
P1 C1 1.844(3) . ?
P1 C11 1.849(3) . ?
P1 C6 1.853(3) . ?
P2 C27 1.835(3) . ?
P2 C22 1.839(3) . ?
P2 C17 1.851(3) . ?
O1 C32 1.156(4) . ?
O2 C33 1.154(4) . ?
O3 C34 1.128(4) . ?
O4 C35 1.147(4) . ?
N1 C5 1.320(4) . ?
N1 C1 1.350(4) . ?
N2 C10 1.313(4) . ?
N2 C6 1.348(4) . ?
N5 C21 1.324(4) . ?
N5 C17 1.342(4) . ?
N6 C26 1.327(4) . ?
N6 C22 1.336(4) . ?
N7 C31 1.310(4) . ?
N7 C27 1.345(4) . ?
C1 C2 1.383(5) . ?
C2 C3 1.366(5) . ?
C3 C4 1.379(5) . ?
C4 C5 1.373(5) . ?
C6 C7 1.381(5) . ?
C7 C8 1.408(5) . ?
C8 C9 1.355(6) . ?
C9 C10 1.372(5) . ?
C11 N4 1.293(9) . ?
C11 C12 1.376(5) . ?
C11 N3 1.452(13) . ?
C12 C13 1.377(5) . ?
C13 C14 1.358(7) . ?
C14 C16 1.264(11) . ?
C14 C15 1.572(14) . ?
C17 C18 1.381(4) . ?
C18 C19 1.392(5) . ?
C19 C20 1.372(5) . ?
C20 C21 1.377(4) . ?
C22 C23 1.400(4) . ?
C23 C24 1.383(5) . ?
C24 C25 1.383(5) . ?
C25 C26 1.384(5) . ?
C27 C28 1.380(4) . ?
C28 C29 1.397(5) . ?
C29 C30 1.366(5) . ?
C30 C31 1.393(5) . ?
Br3 C15 1.847(13) . ?
N3 C15 1.285(15) . ?
Br4 C16 1.926(9) . ?
N4 C16 1.341(11) . ?

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
C33 Mo1 C35 87.63(15) . . ?
C33 Mo1 C32 87.06(15) . . ?
C35 Mo1 C32 88.71(16) . . ?
C33 Mo1 C34 86.71(15) . . ?
C35 Mo1 C34 85.57(16) . . ?
C32 Mo1 C34 171.71(15) . . ?
C33 Mo1 P2 85.57(9) . . ?
C35 Mo1 P2 172.95(11) . . ?
C32 Mo1 P2 92.79(9) . . ?
C34 Mo1 P2 92.18(9) . . ?
C33 Mo1 P1 178.35(11) . . ?
C35 Mo1 P1 91.71(12) . . ?
C32 Mo1 P1 91.41(10) . . ?
C34 Mo1 P1 94.76(10) . . ?
P2 Mo1 P1 95.13(3) . . ?
C1 P1 C11 101.12(16) . . ?
C1 P1 C6 99.41(14) . . ?
C11 P1 C6 97.63(15) . . ?
C1 P1 Mo1 117.91(11) . . ?
C11 P1 Mo1 120.78(11) . . ?
C6 P1 Mo1 116.03(12) . . ?
C27 P2 C22 105.25(14) . . ?
C27 P2 C17 103.22(14) . . ?
C22 P2 C17 98.24(14) . . ?
C27 P2 Mo1 112.52(10) . . ?
C22 P2 Mo1 120.25(9) . . ?
C17 P2 Mo1 115.18(10) . . ?
C5 N1 C1 116.8(3) . . ?
C10 N2 C6 116.6(3) . . ?
C21 N5 C17 117.2(3) . . ?
C26 N6 C22 116.1(3) . . ?
C31 N7 C27 117.7(3) . . ?
N1 C1 C2 122.0(3) . . ?
N1 C1 P1 113.8(2) . . ?
C2 C1 P1 124.1(3) . . ?
C3 C2 C1 118.9(3) . . ?
C2 C3 C4 120.3(3) . . ?
C5 C4 C3 116.4(3) . . ?
N1 C5 C4 125.6(3) . . ?
N1 C5 Br1 115.5(2) . . ?
C4 C5 Br1 118.9(3) . . ?
N2 C6 C7 122.3(3) . . ?
N2 C6 P1 113.4(2) . . ?
C7 C6 P1 124.3(3) . . ?
C6 C7 C8 118.2(3) . . ?
C9 C8 C7 119.7(4) . . ?
C8 C9 C10 116.9(3) . . ?
N2 C10 C9 126.3(3) . . ?
N2 C10 Br2 115.2(3) . . ?
C9 C10 Br2 118.5(3) . . ?
N4 C11 C12 121.1(5) . . ?
C12 C11 N3 126.4(5) . . ?
N4 C11 P1 119.8(4) . . ?
C12 C11 P1 119.1(3) . . ?
N3 C11 P1 112.8(5) . . ?
C11 C12 C13 118.0(4) . . ?
C14 C13 C12 119.5(4) . . ?
C16 C14 C13 116.0(6) . . ?
C13 C14 C15 119.8(5) . . ?
N5 C17 C18 122.4(3) . . ?
N5 C17 P2 113.7(2) . . ?
C18 C17 P2 123.9(2) . . ?
C17 C18 C19 118.9(3) . . ?
C20 C19 C18 119.0(3) . . ?
C19 C20 C21 117.7(3) . . ?
N5 C21 C20 124.8(3) . . ?
N5 C21 Br5 114.4(2) . . ?
C20 C21 Br5 120.8(2) . . ?
N6 C22 C23 123.2(3) . . ?
N6 C22 P2 120.9(2) . . ?
C23 C22 P2 115.8(2) . . ?
C24 C23 C22 118.3(3) . . ?
C23 C24 C25 119.6(3) . . ?
C24 C25 C26 116.7(3) . . ?
N6 C26 C25 126.0(3) . . ?
N6 C26 Br6 116.5(2) . . ?
C25 C26 Br6 117.5(3) . . ?
N7 C27 C28 121.7(3) . . ?
N7 C27 P2 112.7(2) . . ?
C28 C27 P2 124.9(2) . . ?
C27 C28 C29 118.9(3) . . ?
C30 C29 C28 119.9(3) . . ?
C29 C30 C31 116.3(3) . . ?
N7 C31 C30 125.5(3) . . ?
N7 C31 Br7 115.7(3) . . ?
C30 C31 Br7 118.8(3) . . ?
O1 C32 Mo1 173.0(3) . . ?
O2 C33 Mo1 178.0(3) . . ?
O3 C34 Mo1 170.8(3) . . ?
O4 C35 Mo1 174.6(3) . . ?
C15 N3 C11 115.5(9) . . ?
N3 C15 C14 119.9(9) . . ?
N3 C15 Br3 118.4(9) . . ?
C14 C15 Br3 121.5(7) . . ?
C11 N4 C16 116.2(7) . . ?
C14 C16 N4 127.8(8) . . ?
C14 C16 Br4 119.0(6) . . ?
N4 C16 Br4 112.6(6) . . ?

_refine_diff_density_max         1.363
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.131

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_added_by_encifer_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1983667'
_audit_update_record             
;
2020-02-12 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;
#------------------------------------------------------------------------------- 
# this cif originates from: 
#------------------------------------------------------------------------------- 
# leipzig university, faculty of chemistry and mineralogy, 
# johannisallee 29, 04103 leipzig, germany 
#------------------------------------------------------------------------------- 

#=============================================================================== 
#_leipzig_data_id data_x2940 
#=============================================================================== 

_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H24 N6 O4 P2 W'
_chemical_formula_sum            'C34 H24 N6 O4 P2 W'
_chemical_formula_weight         826.38

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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   17.0942(2)
_cell_length_b                   10.26260(10)
_cell_length_c                   17.9547(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3149.81(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    130.00(14)
_cell_measurement_reflns_used    45292
_cell_measurement_theta_min      3.0870
_cell_measurement_theta_max      34.8840

_exptl_crystal_description       block
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_F_000             1624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1500
_exptl_crystal_size_mid          0.1000
_exptl_crystal_size_min          0.1000
_exptl_absorpt_coefficient_mu    3.819
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83776
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130.00(14)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3560
_diffrn_reflns_number            75112
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.269
_diffrn_reflns_theta_max         34.892
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13030
_reflns_number_gt                12313
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_max     0.927
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 4'
_computing_publication_material  SHELXL

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0126P)²+1.5156P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 5586 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.0194(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         13030
_refine_ls_number_parameters     424
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0177
_refine_ls_wR_factor_ref         0.0369
_refine_ls_wR_factor_gt          0.0360
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.007
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.90318(2) 0.06688(2) 0.31619(2) 0.01071(2) Uani 1 1 d . . . . .
O1 O 0.92259(14) 0.3521(2) 0.38316(13) 0.0287(4) Uani 1 1 d . . . . .
P1 P 0.77855(3) 0.12253(6) 0.24770(3) 0.01240(10) Uani 1 1 d . . . . .
P2 P 0.84555(4) 0.01356(6) 0.44079(3) 0.01305(10) Uani 1 1 d . . . . .
O2 O 1.06457(12) -0.0330(2) 0.37635(12) 0.0294(5) Uani 1 1 d . . . . .
N1 N 0.61942(13) 0.0853(2) 0.24326(13) 0.0193(4) Uani 1 1 d . . . . .
N2 N 0.77084(13) -0.0457(2) 0.13285(13) 0.0184(4) Uani 1 1 d . . . . .
N3 N 0.82307(13) 0.3674(2) 0.23020(14) 0.0209(4) Uani 1 1 d . . . . .
O3 O 0.88838(12) -0.21607(18) 0.24556(12) 0.0224(4) Uani 1 1 d . . . . .
N4 N 0.84060(14) -0.2417(2) 0.41319(12) 0.0194(4) Uani 1 1 d . . . . .
O4 O 0.99482(12) 0.1680(2) 0.17590(12) 0.0263(4) Uani 1 1 d . . . . .
N5 N 0.71115(14) 0.1498(2) 0.42201(14) 0.0232(4) Uani 1 1 d . . . . .
N6 N 0.85554(14) 0.1939(2) 0.55153(13) 0.0191(4) Uani 1 1 d . . . . .
C7 C 0.68706(14) 0.0340(2) 0.26807(13) 0.0153(4) Uani 1 1 d . . . . .
C8 C 0.69049(14) -0.0831(2) 0.30750(18) 0.0185(5) Uani 1 1 d . . . . .
H8 H 0.7383 -0.1175 0.3225 0.022 Uiso 1 1 calc R U . . .
C9 C 0.62099(15) -0.1470(3) 0.32378(19) 0.0227(5) Uani 1 1 d . . . . .
H9 H 0.6215 -0.2263 0.3489 0.027 Uiso 1 1 calc R U . . .
C10 C 0.55075(16) -0.0911(3) 0.30215(15) 0.0255(6) Uani 1 1 d . . . . .
H10 H 0.5033 -0.1294 0.3149 0.031 Uiso 1 1 calc R U . . .
C11 C 0.55292(15) 0.0228(3) 0.26113(16) 0.0233(5) Uani 1 1 d . . . . .
H11 H 0.5058 0.0582 0.2450 0.028 Uiso 1 1 calc R U . . .
C12 C 0.79001(14) 0.0771(2) 0.14872(13) 0.0144(4) Uani 1 1 d . . . . .
C13 C 0.82325(18) 0.1619(3) 0.09644(15) 0.0227(5) Uani 1 1 d . . . . .
H13 H 0.8374 0.2462 0.1097 0.027 Uiso 1 1 calc R U . . .
C14 C 0.83458(19) 0.1172(3) 0.02438(16) 0.0261(6) Uani 1 1 d . . . . .
H14 H 0.8560 0.1714 -0.0118 0.031 Uiso 1 1 calc R U . . .
C15 C 0.81356(16) -0.0095(3) 0.00720(15) 0.0222(5) Uani 1 1 d . . . . .
H15 H 0.8199 -0.0417 -0.0408 0.027 Uiso 1 1 calc R U . . .
C16 C 0.78282(16) -0.0873(3) 0.06297(15) 0.0216(5) Uani 1 1 d . . . . .
H16 H 0.7698 -0.1729 0.0513 0.026 Uiso 1 1 calc R U . . .
C17 C 0.75702(14) 0.2989(2) 0.24058(13) 0.0148(4) Uani 1 1 d . . . . .
C18 C 0.68370(15) 0.3576(3) 0.24251(17) 0.0227(5) Uani 1 1 d . . . . .
H18 H 0.6388 0.3082 0.2500 0.027 Uiso 1 1 calc R U . . .
C19 C 0.67899(17) 0.4924(3) 0.23291(18) 0.0270(6) Uani 1 1 d . . . . .
H19 H 0.6307 0.5340 0.2340 0.032 Uiso 1 1 calc R U . . .
C20 C 0.74651(18) 0.5636(3) 0.22184(17) 0.0245(5) Uani 1 1 d . . . . .
H20 H 0.7449 0.6534 0.2152 0.029 Uiso 1 1 calc R U . . .
C21 C 0.81718(17) 0.4961(3) 0.22101(17) 0.0240(5) Uani 1 1 d . . . . .
H21 H 0.8629 0.5435 0.2136 0.029 Uiso 1 1 calc R U . . .
C22 C 0.85491(14) -0.1583(2) 0.46925(13) 0.0154(4) Uani 1 1 d . . . . .
C23 C 0.87563(16) -0.1991(3) 0.54009(14) 0.0197(5) Uani 1 1 d . . . . .
H23 H 0.8826 -0.1390 0.5783 0.024 Uiso 1 1 calc R U . . .
C24 C 0.88579(17) -0.3315(3) 0.55310(16) 0.0228(5) Uani 1 1 d . . . . .
H24 H 0.9003 -0.3613 0.6000 0.027 Uiso 1 1 calc R U . . .
C25 C 0.87408(18) -0.4181(3) 0.49538(17) 0.0228(5) Uani 1 1 d . . . . .
H25 H 0.8820 -0.5070 0.5021 0.027 Uiso 1 1 calc R U . . .
C26 C 0.85006(18) -0.3685(3) 0.42667(16) 0.0239(5) Uani 1 1 d . . . . .
H26 H 0.8401 -0.4270 0.3883 0.029 Uiso 1 1 calc R U . . .
C27 C 0.74255(14) 0.0515(2) 0.46219(14) 0.0158(4) Uani 1 1 d . . . . .
C28 C 0.70097(17) -0.0191(3) 0.51328(18) 0.0292(6) Uani 1 1 d . . . . .
H28 H 0.7249 -0.0851 0.5406 0.035 Uiso 1 1 calc R U . . .
C29 C 0.62263(19) 0.0096(4) 0.5235(2) 0.0385(8) Uani 1 1 d . . . . .
H29 H 0.5932 -0.0371 0.5579 0.046 Uiso 1 1 calc R U . . .
C30 C 0.58867(17) 0.1072(4) 0.48258(19) 0.0329(7) Uani 1 1 d . . . . .
H30 H 0.5358 0.1266 0.4881 0.039 Uiso 1 1 calc R U . . .
C31 C 0.63443(18) 0.1760(3) 0.43308(18) 0.0284(6) Uani 1 1 d . . . . .
H31 H 0.6116 0.2434 0.4061 0.034 Uiso 1 1 calc R U . . .
C32 C 0.89587(14) 0.0991(2) 0.51759(13) 0.0144(4) Uani 1 1 d . . . . .
C33 C 0.97274(15) 0.0679(3) 0.53628(14) 0.0188(5) Uani 1 1 d . . . . .
H33 H 0.9995 0.0029 0.5107 0.023 Uiso 1 1 calc R U . . .
C34 C 1.00851(15) 0.1355(3) 0.59376(15) 0.0204(5) Uani 1 1 d . . . . .
H34 H 1.0592 0.1151 0.6084 0.024 Uiso 1 1 calc R U . . .
C35 C 0.96731(15) 0.2341(3) 0.62898(14) 0.0207(5) Uani 1 1 d . . . . .
H35 H 0.9901 0.2820 0.6672 0.025 Uiso 1 1 calc R U . . .
C36 C 0.89178(16) 0.2599(3) 0.60629(16) 0.0212(5) Uani 1 1 d . . . . .
H36 H 0.8645 0.3263 0.6301 0.025 Uiso 1 1 calc R U . . .
C37 C 0.91455(15) 0.2496(3) 0.35899(15) 0.0176(4) Uani 1 1 d . . . . .
C38 C 1.00460(15) 0.0073(3) 0.35637(14) 0.0175(4) Uani 1 1 d . . . . .
C39 C 0.89138(14) -0.1155(2) 0.27275(14) 0.0150(4) Uani 1 1 d . . . . .
C40 C 0.95986(14) 0.1284(2) 0.22568(14) 0.0166(4) 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
W1 C38 1.975(2) . ?
W1 C40 1.995(2) . ?
W1 C37 2.036(3) . ?
W1 C39 2.038(3) . ?
W1 P2 2.5049(6) . ?
W1 P1 2.5254(6) . ?
O1 C37 1.146(3) . ?
P1 C7 1.845(2) . ?
P1 C12 1.848(2) . ?
P1 C17 1.852(2) . ?
P2 C22 1.843(3) . ?
P2 C27 1.844(2) . ?
P2 C32 1.847(2) . ?
O2 C38 1.162(3) . ?
N1 C11 1.344(3) . ?
N1 C7 1.346(3) . ?
N2 C12 1.334(3) . ?
N2 C16 1.341(3) . ?
N3 C21 1.335(4) . ?
N3 C17 1.343(3) . ?
O3 C39 1.143(3) . ?
N4 C26 1.333(3) . ?
N4 C22 1.344(3) . ?
O4 C40 1.149(3) . ?
N5 C27 1.351(3) . ?
N5 C31 1.354(4) . ?
N6 C32 1.339(3) . ?
N6 C36 1.345(3) . ?
C7 C8 1.396(4) . ?
C8 C9 1.388(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.386(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.383(4) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.400(4) . ?
C13 C14 1.386(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.383(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.384(4) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C18 1.391(3) . ?
C18 C19 1.396(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.380(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.393(4) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.385(3) . ?
C23 C24 1.389(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.380(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.396(4) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C28 1.369(4) . ?
C28 C29 1.383(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.372(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.379(5) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 C33 1.394(3) . ?
C33 C34 1.386(4) . ?
C33 H33 0.9300 . ?
C34 C35 1.385(4) . ?
C34 H34 0.9300 . ?
C35 C36 1.379(4) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C38 W1 C40 88.23(10) . . ?
C38 W1 C37 93.65(10) . . ?
C40 W1 C37 88.26(10) . . ?
C38 W1 C39 86.69(10) . . ?
C40 W1 C39 91.54(10) . . ?
C37 W1 C39 179.60(11) . . ?
C38 W1 P2 87.21(8) . . ?
C40 W1 P2 171.06(7) . . ?
C37 W1 P2 84.36(8) . . ?
C39 W1 P2 95.87(7) . . ?
C38 W1 P1 171.31(7) . . ?
C40 W1 P1 86.64(7) . . ?
C37 W1 P1 93.21(7) . . ?
C39 W1 P1 86.44(7) . . ?
P2 W1 P1 98.77(2) . . ?
C7 P1 C12 99.00(11) . . ?
C7 P1 C17 109.05(11) . . ?
C12 P1 C17 101.61(11) . . ?
C7 P1 W1 120.48(8) . . ?
C12 P1 W1 108.78(8) . . ?
C17 P1 W1 114.99(8) . . ?
C22 P2 C27 103.15(11) . . ?
C22 P2 C32 101.97(11) . . ?
C27 P2 C32 100.87(11) . . ?
C22 P2 W1 114.99(8) . . ?
C27 P2 W1 121.03(8) . . ?
C32 P2 W1 112.31(8) . . ?
C11 N1 C7 117.5(2) . . ?
C12 N2 C16 117.6(2) . . ?
C21 N3 C17 118.1(2) . . ?
C26 N4 C22 117.6(2) . . ?
C27 N5 C31 117.1(3) . . ?
C32 N6 C36 117.5(2) . . ?
N1 C7 C8 122.7(2) . . ?
N1 C7 P1 118.04(19) . . ?
C8 C7 P1 119.25(19) . . ?
C9 C8 C7 118.5(2) . . ?
C9 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?
C10 C9 C8 119.1(3) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C11 C10 C9 118.4(2) . . ?
C11 C10 H10 120.8 . . ?
C9 C10 H10 120.8 . . ?
N1 C11 C10 123.6(3) . . ?
N1 C11 H11 118.2 . . ?
C10 C11 H11 118.2 . . ?
N2 C12 C13 122.9(2) . . ?
N2 C12 P1 114.71(18) . . ?
C13 C12 P1 122.09(19) . . ?
C14 C13 C12 118.5(3) . . ?
C14 C13 H13 120.8 . . ?
C12 C13 H13 120.8 . . ?
C15 C14 C13 118.9(3) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C14 C15 C16 118.6(2) . . ?
C14 C15 H15 120.7 . . ?
C16 C15 H15 120.7 . . ?
N2 C16 C15 123.5(3) . . ?
N2 C16 H16 118.3 . . ?
C15 C16 H16 118.3 . . ?
N3 C17 C18 122.3(2) . . ?
N3 C17 P1 110.74(17) . . ?
C18 C17 P1 126.93(19) . . ?
C17 C18 C19 118.6(3) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
C20 C19 C18 119.6(3) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C19 C20 C21 117.6(3) . . ?
C19 C20 H20 121.2 . . ?
C21 C20 H20 121.2 . . ?
N3 C21 C20 123.8(3) . . ?
N3 C21 H21 118.1 . . ?
C20 C21 H21 118.1 . . ?
N4 C22 C23 122.8(2) . . ?
N4 C22 P2 112.71(18) . . ?
C23 C22 P2 124.5(2) . . ?
C22 C23 C24 118.8(2) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 H23 120.6 . . ?
C25 C24 C23 119.0(3) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C24 C25 C26 118.2(3) . . ?
C24 C25 H25 120.9 . . ?
C26 C25 H25 120.9 . . ?
N4 C26 C25 123.5(3) . . ?
N4 C26 H26 118.3 . . ?
C25 C26 H26 118.3 . . ?
N5 C27 C28 123.2(2) . . ?
N5 C27 P2 115.20(19) . . ?
C28 C27 P2 121.6(2) . . ?
C27 C28 C29 118.6(3) . . ?
C27 C28 H28 120.7 . . ?
C29 C28 H28 120.7 . . ?
C30 C29 C28 119.6(3) . . ?
C30 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?
C29 C30 C31 118.7(3) . . ?
C29 C30 H30 120.7 . . ?
C31 C30 H30 120.7 . . ?
N5 C31 C30 122.9(3) . . ?
N5 C31 H31 118.6 . . ?
C30 C31 H31 118.6 . . ?
N6 C32 C33 122.9(2) . . ?
N6 C32 P2 116.44(18) . . ?
C33 C32 P2 120.62(19) . . ?
C34 C33 C32 118.7(2) . . ?
C34 C33 H33 120.7 . . ?
C32 C33 H33 120.7 . . ?
C35 C34 C33 118.8(2) . . ?
C35 C34 H34 120.6 . . ?
C33 C34 H34 120.6 . . ?
C36 C35 C34 118.8(2) . . ?
C36 C35 H35 120.6 . . ?
C34 C35 H35 120.6 . . ?
N6 C36 C35 123.4(2) . . ?
N6 C36 H36 118.3 . . ?
C35 C36 H36 118.3 . . ?
O1 C37 W1 178.6(2) . . ?
O2 C38 W1 175.8(2) . . ?
O3 C39 W1 175.9(2) . . ?
O4 C40 W1 176.4(2) . . ?

_refine_diff_density_max         1.821
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.082

