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_7008975
_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         'C42 H98 Mo4 Nb2 O22'
_chemical_formula_sum            'C42 H98 Mo4 Nb2 O22'
_chemical_formula_weight         1524.78
_chemical_name_systematic
tetramolybdenumdiniobiumoctaoxotetradecaisopropoxide
_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                94.154(2)
_cell_angle_beta                 93.941(2)
_cell_angle_gamma                107.329(2)
_cell_formula_units_Z            1
_cell_length_a                   10.0293(12)
_cell_length_b                   10.9976(13)
_cell_length_c                   15.7176(18)
_cell_measurement_reflns_used    '999 with I>10sigma(I) '
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      1.30
_cell_volume                     1643.1(3)
_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 0.869
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device_type  'Bruker SMART CCD 1K '
_diffrn_measurement_method       'Bruker SMART '
_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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.1236
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9739
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_T_max  0.8477
_exptl_absorpt_correction_T_min  0.5247
_exptl_absorpt_correction_type   'Bruker SADABS '
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.00031(16)
_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   0.808
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         7114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.808
_refine_ls_R_factor_all          0.1403
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          3.448
_refine_ls_shift/su_mean         0.046
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                3116
_reflns_number_total             7114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a907720k.txt
_cod_data_source_block           monb1m
_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               7008975