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_4507443
_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         'C28 H44 Cu5 I3 N8 S4 W'
_chemical_formula_sum            'C28 H44 Cu5 I3 N8 S4 W'
_chemical_formula_weight         1503.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 92.9894(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4014(2)
_cell_length_b                   16.5049(3)
_cell_length_c                   12.6499(2)
_cell_measurement_reflns_used    4526
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      62.01
_cell_measurement_theta_min      2.68
_cell_volume                     2168.70(7)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_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 Ultra optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6254
_diffrn_reflns_theta_full        62.10
_diffrn_reflns_theta_max         62.10
_diffrn_reflns_theta_min         3.50
_exptl_absorpt_coefficient_mu    26.242
_exptl_absorpt_correction_T_max  0.780
_exptl_absorpt_correction_T_min  0.077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.166
_refine_diff_density_min         -1.769
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       0.00005(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+3.2637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                3137
_reflns_number_total             3482
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cg301106g_si_002.cif
_cod_data_source_block           ab102_1
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4507443
_computing_special_details
;
TITL ab102 in P2(1)/m
CELL  1.54178   10.4014   16.5049   12.6499    90.000    92.9894    90.000
ZERR  2          0.0002    0.0003    0.0002     0.000     0.0017     0.000
LATT 1
SYMM -X, 0.5+Y, -Z
SFAC C H CU I N S W
UNIT 56 88 10 6 16 8 2

REM red rod
SIZE 0.20 0.01 0.01
TEMP -123
REM SHEL 5.8 1.0
OMIT  -6  15   1
OMIT  -6  13   1

L.S. 8
ACTA
BOND $H
FMAP 2
PLAN 10

WGHT    0.071500    3.263700
EXTI    0.000054
FVAR       0.17612
W     7    0.820104    0.250000    0.119012    10.50000    0.01553    0.02243 =
         0.01167    0.00000   -0.00242    0.00000
S1    6    0.996848    0.250000    0.025118    10.50000    0.01804    0.03049 =
         0.01898    0.00000   -0.00095    0.00000
S2    6    0.700648    0.360563    0.078079    11.00000    0.02069    0.02391 =
         0.01397    0.00138   -0.00053    0.00091
S3    6    0.870999    0.250000    0.292165    10.50000    0.02071    0.03052 =
         0.01505    0.00000   -0.00598    0.00000
CU1   3    0.864450    0.352957   -0.040123    11.00000    0.02608    0.03482 =
         0.02827    0.01072    0.00700    0.00354
CU2   3    0.594261    0.250000    0.002081    10.50000    0.02643    0.03309 =
         0.06141    0.00000   -0.02215    0.00000
CU3   3    0.712023    0.347112    0.261899    11.00000    0.02888    0.02761 =
         0.01502   -0.00313   -0.00293    0.00297
I1    4    0.721510    0.250000   -0.199904    10.50000    0.03206    0.04048 =
         0.01655    0.00000   -0.00208    0.00000
I2    4    0.361964    0.250000   -0.048438    10.50000    0.02001    0.03831 =
         0.03900    0.00000   -0.00817    0.00000
I3    4    0.500598    0.250000    0.303924    10.50000    0.02317    0.02414 =
         0.02812    0.00000    0.00422    0.00000
N1    5    0.693775    0.440059    0.356671    11.00000    0.02752    0.02591 =
         0.01547   -0.00187    0.00185   -0.00264
N2    5    0.632855    0.511452    0.331051    11.00000    0.02969    0.02460 =
         0.02394   -0.00622    0.00356   -0.00108
N3    5    0.149223    0.486012    0.148114    11.00000    0.02708    0.02668 =
         0.02433    0.00219   -0.00119   -0.00235
N4    5    0.086340    0.558388    0.133408    11.00000    0.02419    0.02151 =
         0.02519    0.00324    0.00138   -0.00020
C1    1    0.802094    0.379256    0.515547    11.00000    0.06178    0.04735 =
         0.01785    0.00182   -0.00467   -0.00004
AFIX 137
H1A   2    0.748068    0.330584    0.512326    11.00000   -1.50000
H1B   2    0.820726    0.394409    0.589673    11.00000   -1.50000
H1C   2    0.882942    0.368263    0.481747    11.00000   -1.50000
AFIX   0
C2    1    0.733885    0.446052    0.459867    11.00000    0.03524    0.03647 =
         0.01722   -0.00217   -0.00113   -0.00627
C3    1    0.698153    0.521532    0.498060    11.00000    0.06165    0.03325 =
         0.01690   -0.00838    0.00624   -0.00753
AFIX  43
H3    2    0.716037    0.541676    0.567627    11.00000   -1.20000
AFIX   0
C4    1    0.632893    0.561175    0.417444    11.00000    0.04962    0.02710 =
         0.03333   -0.01072    0.00643   -0.00444
C5    1    0.570040    0.641718    0.409815    11.00000    0.09341    0.03592 =
         0.04925   -0.00872    0.00855    0.01322
AFIX 137
H5A   2    0.480763    0.635344    0.382355    11.00000   -1.50000
H5B   2    0.616623    0.676390    0.361891    11.00000   -1.50000
H5C   2    0.571181    0.666670    0.480157    11.00000   -1.50000
AFIX   0
C6    1    0.569073    0.523945    0.228845    11.00000    0.03165    0.02852 =
         0.01931    0.00493    0.00682    0.00288
AFIX  23
H6A   2    0.623877    0.501962    0.173949    11.00000   -1.20000
H6B   2    0.559584    0.582899    0.216293    11.00000   -1.20000
AFIX   0
C7    1    0.437163    0.484534    0.216800    11.00000    0.02775    0.02694 =
         0.02562    0.00542    0.00447   -0.00001
AFIX  23
H7A   2    0.444866    0.425860    0.232104    11.00000   -1.20000
H7B   2    0.379587    0.508700    0.268141    11.00000   -1.20000
AFIX   0
C8    1    0.380221    0.496690    0.105682    11.00000    0.02653    0.04505 =
         0.02794    0.00552    0.00549    0.00669
AFIX  23
H8A   2    0.441631    0.474459    0.055962    11.00000   -1.20000
H8B   2    0.374008    0.555710    0.092424    11.00000   -1.20000
AFIX   0
C9    1    0.248968    0.459632    0.078232    11.00000    0.03946    0.03434 =
         0.02305   -0.00574    0.00262    0.00171
AFIX  23
H9A   2    0.222140    0.474209    0.004433    11.00000   -1.20000
H9B   2    0.256368    0.399888    0.081948    11.00000   -1.20000
AFIX   0
C10   1    0.155949    0.364196    0.264879    11.00000    0.02772    0.02562 =
         0.03493    0.00065   -0.00487   -0.00744
AFIX 137
H10A  2    0.248887    0.368225    0.281120    11.00000   -1.50000
H10B  2    0.139378    0.324996    0.207593    11.00000   -1.50000
H10C  2    0.113279    0.346219    0.328041    11.00000   -1.50000
AFIX   0
C11   1    0.104561    0.445242    0.231151    11.00000    0.02024    0.02996 =
         0.02570    0.00492   -0.00538   -0.00899
C12   1    0.008971    0.491672    0.270290    11.00000    0.02399    0.03682 =
         0.02661    0.00777    0.00113   -0.00587
AFIX  43
H12   2   -0.042241    0.478650    0.327952    11.00000   -1.20000
AFIX   0
C13   1    0.001518    0.561619    0.209121    11.00000    0.02305    0.03626 =
         0.02499    0.00649    0.00120   -0.00096
C14   1   -0.084082    0.632255    0.221358    11.00000    0.04521    0.04306 =
         0.04829    0.01544    0.01976    0.01285
AFIX 137
H14A  2   -0.136266    0.640745    0.155536    11.00000   -1.50000
H14B  2   -0.031915    0.680621    0.237184    11.00000   -1.50000
H14C  2   -0.140747    0.622175    0.279457    11.00000   -1.50000

HKLF 4

REM  ab102 in P2(1)/m
REM R1 =  0.0351 for   3137 Fo > 4sig(Fo)  and  0.0398 for all   3482 data
REM    237 parameters refined using      0 restraints

END

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