The solution thermolysis approach to molybdenum(V) alkoxides: synthesis, solid state and solution structures of the bimetallic alkoxides of molybdenum(V) and niobium(V), tantalum(V) and tungsten(VI)
Johansson, Anders; Roman, Magnus; Seisenbaeva, Gulaim A.; Kloo, Lars; Szabo, Zoltan; Kessler, Vadim G.; Journal of the Chemical Society, Dalton Transactions  (2000) 387–; doi:10.1039/a907720k

data_7008976
_publ_section_title
;
 The solution thermolysis approach to molybdenum(V) alkoxides:
 synthesis, solid state and solution structures of the bimetallic
 alkoxides of molybdenum(V) and niobium(V), tantalum(V) and
 tungsten(VI)
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              387
_journal_paper_doi               10.1039/a907720k
_journal_year                    2000
_chemical_formula_moiety         'C21 H49 Mo2 O11 Ta'
_chemical_formula_sum            'C42 H98 Mo4 O22 Ta2'
_chemical_formula_weight         1700.86
_chemical_name_common            ' Molybdenum-tantalum oxoisopropoxide '
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                94.159(5)
_cell_angle_beta                 94.091(7)
_cell_angle_gamma                107.143(4)
_cell_formula_units_Z            2
_cell_length_a                   10.0444(17)
_cell_length_b                   11.0070(19)
_cell_length_c                   15.769(3)
_cell_measurement_reflns_used    '998 with I > 10 sigma(I) '
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      1.30
_cell_volume                     1653.7(5)
_computing_cell_refinement       ' Bruker SMART '
_computing_data_collection       ' Bruker SMART '
_computing_data_reduction        ' Bruker SAINTPLUS'
_computing_molecular_graphics    ' Bruker SHELXTL 5.3  '
_computing_publication_material  ' Bruker SHELXTL 5.3  '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.862
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  ' SMART CCD'
_diffrn_measurement_method       'CCD area Detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.1122
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9792
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    4.091
_exptl_absorpt_correction_T_max  0.4950
_exptl_absorpt_correction_T_min  0.1927
_exptl_absorpt_correction_type   'Bruker SADABS '
_exptl_absorpt_process_details   ' Bruker SADABS '
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             840
_exptl_crystal_size_max          '0.60 mm '
_exptl_crystal_size_mid          '0.50 mm '
_exptl_crystal_size_min          '0.20 mm '
_refine_diff_density_max         0.899
_refine_diff_density_min         -2.175
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.737
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         7141
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.737
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.080
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                3909
_reflns_number_total             7141
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a907720k.txt
_cod_data_source_block           tamopr2t
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7008976