Metal-to-Ligand Ratio As a Design Factor in the One-Pot Synthesis of Coordination Polymers with [MS4Cun] (M = W or Mo,n= 3 or 5) Cluster Nodes and a Flexible Pyrazole-Based Bridging Ligand
Beheshti, Azizolla; Clegg, William; Nobakht, Valiollah; Harrington, Ross W.; Crystal Growth & Design 13 (2013) 1023–; doi:10.1021/cg301106g

data_4507444
_publ_section_title
;
 Metal-to-Ligand Ratio As a Design Factor in the One-Pot Synthesis of
 Coordination Polymers with [MS4Cun] (M = W or Mo,n= 3 or 5) Cluster Nodes
 and a Flexible Pyrazole-Based Bridging Ligand
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1023
_journal_paper_doi               10.1021/cg301106g
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         'C42 H66 Cu6 I2 N12 S8 W2,C3 H7 N O'
_chemical_formula_sum            'C45 H73 Cu6 I2 N13 O S8 W2'
_chemical_formula_weight         2071.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.561(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.1170(11)
_cell_length_b                   18.9892(14)
_cell_length_c                   16.9251(10)
_cell_measurement_reflns_used    5375
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      2.89
_cell_volume                     6445.0(7)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type
'Oxford Diffraction Gemini A Ultra diffractometer'
_diffrn_measurement_method       'thick-slice \w scans'
_diffrn_radiation_monochromator  none
_diffrn_radiation_source         'sealed tube with Enhance optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1217
_diffrn_reflns_av_sigmaI/netI    0.1381
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45441
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    6.755
_exptl_absorpt_correction_T_max  0.552
_exptl_absorpt_correction_T_min  0.431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3992
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.790
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.263
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         10899
_refine_ls_number_restraints     509
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                6865
_reflns_number_total             10899
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cg301106g_si_002.cif
_cod_data_source_block           ab104_2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4507444
_computing_special_details
;
TITL ab104 in P2(1)/c
CELL 0.71073  20.1170  18.9892  16.9251  90.000  94.561  90.000
ZERR    4.00   0.0011   0.0014   0.0010   0.000   0.005   0.000
LATT  1
SYMM -X, 0.5+Y, 0.5-Z
SFAC C H O S CU W  N I
UNIT 180 292 4 32 24  8 52 8

REM orange block
SIZE 0.15 0.1 0.1
TEMP -123
OMIT -3 50
OMIT -3   1   9
OMIT -1   4   2
OMIT  1  14   3

L.S. 20
ACTA
BOND $H
BIND I2 CU4
FMAP 2
PLAN 10

SIMU 0.005 $C $N $O
DELU 0.005 $C $N $O

REM EXTI    0.000000
WGHT    0.000000
FVAR       0.03797
W1    6    0.118074    0.592657    0.318410    11.00000    0.02043    0.01769 =
         0.02004    0.00284    0.00509   -0.00070
S1    4    0.069485    0.494919    0.263996    11.00000    0.02029    0.02285 =
         0.02267    0.00191    0.00013   -0.00231
S2    4    0.199048    0.559201    0.409232    11.00000    0.02990    0.01883 =
         0.01368    0.00160    0.00264   -0.00437
S3    4    0.165222    0.651986    0.223536    11.00000    0.02848    0.02154 =
         0.01781    0.00488    0.00117   -0.00423
S4    4    0.048123    0.658502    0.372510    11.00000    0.03909    0.03205 =
         0.05095    0.00342    0.01850    0.00222
CU1   5    0.127308    0.547573    0.169488    11.00000    0.04603    0.03267 =
         0.01908   -0.00319    0.00616   -0.01168
CU2   5    0.159683    0.460549    0.344893    11.00000    0.02761    0.01770 =
         0.02412    0.00162   -0.00459   -0.00125
CU3   5    0.249990    0.603564    0.303199    11.00000    0.02161    0.02631 =
         0.02150    0.00644    0.00051   -0.00641
I1    8    0.257462    0.468348    0.219942    11.00000    0.02946    0.03408 =
         0.02113   -0.00190    0.00574    0.00570
W2    6    0.387897    0.545843    0.695901    11.00000    0.01867    0.01549 =
         0.01440   -0.00115    0.00161    0.00109
S5    4    0.349386    0.577175    0.811698    11.00000    0.02256    0.02053 =
         0.01392   -0.00483   -0.00133    0.00441
S6    4    0.301694    0.535313    0.605112    11.00000    0.01892    0.02085 =
         0.01654    0.00033    0.00208    0.00255
S7    4    0.437593    0.439996    0.711238    11.00000    0.02005    0.02031 =
         0.01775   -0.00080    0.00184    0.00731
S8    4    0.455170    0.624451    0.658910    11.00000    0.03147    0.03140 =
         0.03228   -0.00076    0.00458   -0.00242
CU4   5    0.396018    0.467625    0.826941    11.00000    0.03296    0.02261 =
         0.01684    0.00033    0.00459    0.00750
CU5   5    0.258323    0.552023    0.725095    11.00000    0.02001    0.02934 =
         0.01618   -0.00637   -0.00003    0.00455
CU6   5    0.338648    0.423869    0.636986    11.00000    0.03257    0.01772 =
         0.02041   -0.00396   -0.00426    0.00185
I2    8    0.247885    0.401938    0.762946    11.00000    0.03472    0.02002 =
         0.02384    0.00263    0.00942   -0.00211
N1    7    0.162381    0.366321    0.389559    11.00000    0.02312    0.01753 =
         0.01588   -0.00329    0.00283   -0.00014
N2    7    0.165206    0.349931    0.469558    11.00000    0.02501    0.01933 =
         0.01722   -0.00297    0.00328   -0.00142
N3    7    0.121543    0.597347    0.665726    11.00000    0.01948    0.02442 =
         0.01664   -0.00369   -0.00026   -0.00501
N4    7    0.172116    0.600190    0.724076    11.00000    0.01792    0.02140 =
         0.01539   -0.00141    0.00119   -0.00662
C1    1    0.163878    0.248728    0.561589    11.00000    0.05387    0.02754 =
         0.02056    0.00184    0.01225   -0.00384
AFIX 137
H1A   2    0.204756    0.262687    0.593047    11.00000   -1.50000
H1B   2    0.162063    0.197276    0.557456    11.00000   -1.50000
H1C   2    0.125020    0.265708    0.587413    11.00000   -1.50000
AFIX   0
C2    1    0.163564    0.279952    0.480682    11.00000    0.03177    0.02013 =
         0.01898   -0.00172    0.00665   -0.00417
C3    1    0.159307    0.249954    0.405835    11.00000    0.03132    0.01966 =
         0.01964   -0.00335    0.00347   -0.00181
AFIX  43
H3    2    0.156603    0.201176    0.393530    11.00000   -1.20000
AFIX   0
C4    1    0.159765    0.303855    0.353873    11.00000    0.03026    0.01878 =
         0.01904   -0.00428    0.00369   -0.00023
C5    1    0.151765    0.299056    0.264489    11.00000    0.04789    0.02607 =
         0.01938   -0.00594    0.00787    0.00303
AFIX 137
H5A   2    0.184206    0.330138    0.241880    11.00000   -1.50000
H5B   2    0.106521    0.313509    0.245515    11.00000   -1.50000
H5C   2    0.159382    0.250408    0.248114    11.00000   -1.50000
AFIX   0
C6    1    0.164202    0.405650    0.528816    11.00000    0.02016    0.02177 =
         0.01663   -0.00450    0.00199   -0.00427
AFIX  23
H6A   2    0.190078    0.446329    0.511299    11.00000   -1.20000
H6B   2    0.186516    0.388371    0.579367    11.00000   -1.20000
AFIX   0
C7    1    0.094763    0.430114    0.543270    11.00000    0.02023    0.02720 =
         0.01854   -0.00624    0.00374   -0.00381
AFIX  23
H7A   2    0.066832    0.388377    0.552181    11.00000   -1.20000
H7B   2    0.075179    0.454303    0.495089    11.00000   -1.20000
AFIX   0
C8    1    0.092322    0.479320    0.613092    11.00000    0.02440    0.02667 =
         0.01977   -0.00596    0.00454   -0.00397
AFIX  23
H8A   2    0.045235    0.487039    0.623935    11.00000   -1.20000
H8B   2    0.115391    0.457026    0.660535    11.00000   -1.20000
AFIX   0
C9    1    0.124167    0.548766    0.598997    11.00000    0.02144    0.02610 =
         0.01676   -0.00458    0.00065   -0.00546
AFIX  23
H9A   2    0.171352    0.540940    0.588661    11.00000   -1.20000
H9B   2    0.101433    0.570638    0.551091    11.00000   -1.20000
AFIX   0
C10   1    0.011800    0.653295    0.620476    11.00000    0.02132    0.02222 =
         0.02819   -0.00078   -0.00535   -0.00288
AFIX 137
H10A  2    0.025848    0.665995    0.568207    11.00000   -1.50000
H10B  2   -0.016343    0.690801    0.639499    11.00000   -1.50000
H10C  2   -0.013524    0.609180    0.616457    11.00000   -1.50000
AFIX   0
C11   1    0.072737    0.643880    0.678085    11.00000    0.02137    0.02362 =
         0.01826   -0.00272   -0.00071   -0.00415
C12   1    0.090999    0.678071    0.747680    11.00000    0.02192    0.02307 =
         0.01803   -0.00243    0.00068   -0.00146
AFIX  43
H12   2    0.066294    0.713224    0.772515    11.00000   -1.20000
AFIX   0
C13   1    0.153478    0.650829    0.774991    11.00000    0.02118    0.02144 =
         0.01759   -0.00243   -0.00057   -0.00235
C14   1    0.193298    0.669182    0.848138    11.00000    0.02459    0.02542 =
         0.02792   -0.01113   -0.00240    0.00107
AFIX 137
H14A  2    0.231752    0.637495    0.855374    11.00000   -1.50000
H14B  2    0.165919    0.664450    0.893217    11.00000   -1.50000
H14C  2    0.208911    0.717900    0.844846    11.00000   -1.50000
AFIX   0
N5    7    0.095122    0.550339    0.056562    11.00000    0.01936    0.03086 =
         0.02006    0.00035    0.00146    0.00008
N6    7    0.111562    0.508790   -0.004572    11.00000    0.01982    0.02693 =
         0.01788    0.00165   -0.00062    0.00026
N7    7    0.415256    0.444760   -0.001512    11.00000    0.02390    0.02217 =
         0.01598    0.00105   -0.00239    0.00620
N8    7    0.432053    0.426842   -0.074334    11.00000    0.02704    0.02289 =
         0.01776    0.00495   -0.00001    0.00860
C15   1    0.018056    0.650666    0.071968    11.00000    0.04059    0.04065 =
         0.04890   -0.00807    0.00853    0.00990
AFIX 137
H15A  2    0.015473    0.634278    0.126544    11.00000   -1.50000
H15B  2   -0.026939    0.660722    0.048137    11.00000   -1.50000
H15C  2    0.045108    0.693591    0.072081    11.00000   -1.50000
AFIX   0
C16   1    0.049515    0.594583    0.024673    11.00000    0.02192    0.03289 =
         0.02660   -0.00018    0.00189    0.00183
C17   1    0.037985    0.582186   -0.055981    11.00000    0.02237    0.03097 =
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AFIX  43
H17   2    0.008300    0.607587   -0.091974    11.00000   -1.20000
AFIX   0
C18   1    0.077752    0.525923   -0.074362    11.00000    0.01902    0.02984 =
         0.02000    0.00245   -0.00319   -0.00330
C19   1    0.089924    0.491247   -0.149260    11.00000    0.02977    0.04590 =
         0.02279   -0.00641   -0.00729   -0.00550
AFIX 137
H19A  2    0.137745    0.492335   -0.156606    11.00000   -1.50000
H19B  2    0.065402    0.515982   -0.193271    11.00000   -1.50000
H19C  2    0.074759    0.442247   -0.147962    11.00000   -1.50000
AFIX   0
C20   1    0.166778    0.458829    0.006620    11.00000    0.02433    0.01981 =
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AFIX  23
H20A  2    0.160915    0.420777   -0.033311    11.00000   -1.20000
H20B  2    0.167165    0.437280    0.059917    11.00000   -1.20000
AFIX   0
C21   1    0.232209    0.496471   -0.001834    11.00000    0.02336    0.01775 =
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AFIX  23
H21A  2    0.239620    0.531278    0.041520    11.00000   -1.20000
H21B  2    0.229286    0.522514   -0.052664    11.00000   -1.20000
AFIX   0
C22   1    0.291647    0.446369    0.000463    11.00000    0.02492    0.01896 =
         0.01024   -0.00020   -0.00197    0.00085
AFIX  23
H22A  2    0.290630    0.414359    0.046521    11.00000   -1.20000
H22B  2    0.289155    0.417393   -0.048309    11.00000   -1.20000
AFIX   0
C23   1    0.356369    0.488577    0.006868    11.00000    0.02614    0.02194 =
         0.01476   -0.00162   -0.00157    0.00313
AFIX  23
H23A  2    0.353939    0.525314   -0.034766    11.00000   -1.20000
H23B  2    0.361114    0.512542    0.058958    11.00000   -1.20000
AFIX   0
C24   1    0.448312    0.430804    0.140806    11.00000    0.02787    0.03759 =
         0.01724   -0.00028   -0.00643   -0.00344
AFIX 137
H24A  2    0.404420    0.413777    0.153487    11.00000   -1.50000
H24B  2    0.451765    0.481397    0.151803    11.00000   -1.50000
H24C  2    0.483165    0.405706    0.173332    11.00000   -1.50000
AFIX   0
C25   1    0.456507    0.418384    0.058364    11.00000    0.02469    0.02539 =
         0.01817    0.00403   -0.00147    0.00348
C26   1    0.504261    0.380572    0.020427    11.00000    0.02574    0.02428 =
         0.02356    0.00592   -0.00177    0.00803
AFIX  43
H26   2    0.541541    0.356428    0.045532    11.00000   -1.20000
AFIX   0
C27   1    0.487865    0.384514   -0.058597    11.00000    0.02826    0.02391 =
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C28   1    0.522413    0.351296   -0.124757    11.00000    0.04197    0.03078 =
         0.03165   -0.00391    0.00825    0.01515
AFIX 137
H28A  2    0.530917    0.387192   -0.164317    11.00000   -1.50000
H28B  2    0.494027    0.314236   -0.149635    11.00000   -1.50000
H28C  2    0.564824    0.330800   -0.103462    11.00000   -1.50000
AFIX   0
N9    7    0.335256    0.345112    0.565224    11.00000    0.02214    0.01373 =
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N10   7    0.334030    0.348894    0.483249    11.00000    0.02401    0.01549 =
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N11   7    0.384720    0.635777    0.376868    11.00000    0.02136    0.01953 =
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N12   7    0.337932    0.648200    0.316002    11.00000    0.01966    0.02336 =
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C29   1    0.347231    0.250248    0.662869    11.00000    0.04566    0.01456 =
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AFIX 137
H29A  2    0.315154    0.276049    0.692551    11.00000   -1.50000
H29B  2    0.392449    0.258437    0.687092    11.00000   -1.50000
H29C  2    0.337165    0.199780    0.664004    11.00000   -1.50000
AFIX   0
C30   1    0.342577    0.275194    0.579536    11.00000    0.02642    0.01362 =
         0.02079   -0.00257    0.00589   -0.00444
C31   1    0.346654    0.238082    0.510096    11.00000    0.02858    0.01330 =
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AFIX  43
H31   2    0.352131    0.188624    0.505198    11.00000   -1.20000
AFIX   0
C32   1    0.341344    0.285731    0.449917    11.00000    0.02792    0.01531 =
         0.02110   -0.00614    0.00402   -0.00377
C33   1    0.345617    0.276423    0.362982    11.00000    0.04664    0.02112 =
         0.02306   -0.00730   -0.00135   -0.00773
AFIX 137
H33A  2    0.305743    0.296380    0.334327    11.00000   -1.50000
H33B  2    0.348580    0.226133    0.350741    11.00000   -1.50000
H33C  2    0.385338    0.300641    0.346746    11.00000   -1.50000
AFIX   0
C34   1    0.335398    0.418055    0.444702    11.00000    0.02432    0.01617 =
         0.01600   -0.00191   -0.00073    0.00097
AFIX  23
H34A  2    0.308639    0.451881    0.473412    11.00000   -1.20000
H34B  2    0.315074    0.414255    0.389646    11.00000   -1.20000
AFIX   0
C35   1    0.406664    0.445443    0.443694    11.00000    0.02615    0.01921 =
         0.02258    0.00206    0.00080    0.00049
AFIX  23
H35A  2    0.423790    0.457368    0.498517    11.00000   -1.20000
H35B  2    0.435152    0.407552    0.424595    11.00000   -1.20000
AFIX   0
C36   1    0.412187    0.509620    0.391730    11.00000    0.02327    0.01983 =
         0.02253    0.00155   -0.00089   -0.00080
AFIX  23
H36A  2    0.389530    0.500011    0.338749    11.00000   -1.20000
H36B  2    0.459809    0.518928    0.384890    11.00000   -1.20000
AFIX   0
C37   1    0.381227    0.574928    0.426761    11.00000    0.02314    0.01934 =
         0.02173    0.00093    0.00064   -0.00179
AFIX  23
H37A  2    0.333941    0.565081    0.434957    11.00000   -1.20000
H37B  2    0.404673    0.585153    0.479159    11.00000   -1.20000
AFIX   0
C38   1    0.490530    0.685655    0.440995    11.00000    0.02476    0.02710 =
         0.02772   -0.00313   -0.00504   -0.00935
AFIX 137
H38A  2    0.518657    0.726994    0.434119    11.00000   -1.50000
H38B  2    0.516829    0.642751    0.435442    11.00000   -1.50000
H38C  2    0.473818    0.686826    0.493810    11.00000   -1.50000
AFIX   0
C39   1    0.434202    0.686242    0.380674    11.00000    0.01949    0.02256 =
         0.02310    0.00119    0.00087   -0.00339
C40   1    0.417626    0.732200    0.318241    11.00000    0.02032    0.02259 =
         0.02235    0.00219    0.00423   -0.00288
AFIX  43
H40   2    0.441907    0.772653    0.304320    11.00000   -1.20000
AFIX   0
C41   1    0.357880    0.706971    0.279838    11.00000    0.01880    0.02438 =
         0.02057    0.00364    0.00442   -0.00279
C42   1    0.319900    0.738744    0.210360    11.00000    0.02949    0.03162 =
         0.02926    0.01287   -0.00148   -0.00894
AFIX 137
H42A  2    0.311241    0.702885    0.169183    11.00000   -1.50000
H42B  2    0.345852    0.777269    0.189600    11.00000   -1.50000
H42C  2    0.277443    0.757128    0.226264    11.00000   -1.50000
AFIX   0
O     3    0.310552    0.643836    0.019630    11.00000    0.05127    0.02987 =
         0.05073   -0.00677    0.00607    0.01194
N13   7    0.248642    0.742811    0.026097    11.00000    0.04555    0.02091 =
         0.03270    0.00367    0.00878    0.00595
C43   1    0.259252    0.672835    0.034405    11.00000    0.04249    0.02089 =
         0.03500    0.00430    0.00915    0.00346
AFIX  43
H43   2    0.224586    0.644769    0.052853    11.00000   -1.20000
AFIX   0
C44   1    0.187655    0.774459    0.048265    11.00000    0.05185    0.02993 =
         0.03814    0.00169    0.01013    0.01168
AFIX 137
H44A  2    0.156669    0.737435    0.062052    11.00000   -1.50000
H44B  2    0.167387    0.802070    0.003732    11.00000   -1.50000
H44C  2    0.197471    0.805373    0.094075    11.00000   -1.50000
AFIX   0
C45   1    0.298866    0.785075   -0.003346    11.00000    0.05052    0.01871 =
         0.03551    0.00316    0.00211    0.00108
AFIX 137
H45A  2    0.330104    0.755146   -0.029637    11.00000   -1.50000
H45B  2    0.322888    0.810316    0.040645    11.00000   -1.50000
H45C  2    0.278467    0.819101   -0.041485    11.00000   -1.50000

HKLF 4

REM  ab104 in P2(1)/c
REM R1 =  0.0591 for   6865 Fo > 4sig(Fo)  and  0.1162 for all  10899 data
REM    708 parameters refined using    509 restraints

END
;