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_7023245
_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         'C32 H70 Mo6 N2 O16 P6 S20'
_chemical_formula_sum            'C32 H70 Mo6 N2 O16 P6 S20'
_chemical_formula_weight         2141.56
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-05-31
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1592(2)
_cell_length_b                   20.8726(4)
_cell_length_c                   25.0380(4)
_cell_measurement_reflns_used    13553
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.2040
_cell_measurement_theta_min      3.7400
_cell_volume                     7399.7(2)
_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
;
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(2)
_diffrn_detector_area_resol_mean 10.5953
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9542
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0404174000
_diffrn_orient_matrix_UB_12      0.0135186000
_diffrn_orient_matrix_UB_13      -0.0560163000
_diffrn_orient_matrix_UB_21      -0.0802615000
_diffrn_orient_matrix_UB_22      0.0396528000
_diffrn_orient_matrix_UB_23      0.0251347000
_diffrn_orient_matrix_UB_31      0.0614329000
_diffrn_orient_matrix_UB_32      0.0607226000
_diffrn_orient_matrix_UB_33      -0.0040314000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            51323
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.598
_diffrn_reflns_theta_min         3.121
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.050
_exptl_absorpt_correction_T_max  0.553
_exptl_absorpt_correction_T_min  0.114
_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    1.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4264
_exptl_crystal_size_max          0.2834
_exptl_crystal_size_mid          0.1309
_exptl_crystal_size_min          0.0431
_refine_diff_density_max         1.357
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.221
_refine_ls_abs_structure_details
;
 Flack x determined using 4590 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.006(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         12757
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0989P)^2^+33.1300P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.1907
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.929
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                10900
_reflns_number_total             12757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt51101d.txt
_cod_data_source_block           Sample6
_cod_database_code               7023245
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49