Tungsten and molybdenum incomplete cuboidal clusters; kinetico-mechanistic studies and association in dimers.
Hernandez-Molina, Rita; Gushchin, Artem; González-Platas, Javier; Martínez, Manuel; Rodríguez, Carlos; Vicent, Cristian; Dalton transactions (Cambridge, England : 2003) 42 (2013) 15016–15027; doi:10.1039/c3dt51101d

data_7023244
_publ_section_title
;
 Tungsten and molybdenum incomplete cuboidal clusters;
 kinetico-mechanistic studies and association in dimers.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15016
_journal_page_last               15027
_journal_paper_doi               10.1039/c3dt51101d
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C14 H34 Mo3 O9 P3 S10, C12 H12 N2, C2 H6 O'
_chemical_formula_sum            'C28 H52 Mo3 N2 O10 P3 S10'
_chemical_formula_weight         1278.04
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-31
_audit_creation_method
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  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                104.542(4)
_cell_angle_beta                 93.902(3)
_cell_angle_gamma                108.054(4)
_cell_formula_units_Z            2
_cell_length_a                   12.8385(4)
_cell_length_b                   13.8201(6)
_cell_length_c                   14.9195(6)
_cell_measurement_reflns_used    21934
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.6655
_cell_measurement_theta_min      3.6675
_cell_volume                     2405.40(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
M.C.Burla, R.Caliandro, M.Camalli, B.Carrozzini, G.L.Cascarano, C.Giacovazzo,
M.Mallamo, A.Mazzone, G.Polidori and R. Spagna
SIR2011: a new package for crystal structure determination and refinement
J. Appl. Cryst. (2012). 45, 357-361.
;
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 10.5953
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9826
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0304238000
_diffrn_orient_matrix_UB_12      -0.0761572000
_diffrn_orient_matrix_UB_13      0.0481727000
_diffrn_orient_matrix_UB_21      0.0357858000
_diffrn_orient_matrix_UB_22      0.0881633000
_diffrn_orient_matrix_UB_23      0.0941133000
_diffrn_orient_matrix_UB_31      -0.1188824000
_diffrn_orient_matrix_UB_32      -0.0375103000
_diffrn_orient_matrix_UB_33      0.0222468000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34841
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_min         3.667
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.730
_exptl_absorpt_correction_T_max  0.406
_exptl_absorpt_correction_T_min  0.116
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1290
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.2004
_exptl_crystal_size_min          0.1197
_refine_diff_density_max         1.113
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         8499
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+3.1970P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0814
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8057
_reflns_number_total             8499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt51101d.txt
_cod_data_source_block           Sample5
_cod_original_cell_volume        2405.41(18)
_cod_database_code               7023244
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97