Electrochemical Synthesis, X-ray Single Crystal, IR Spectroscopic, and Quantum Chemical Investigation of Molybdenum and Tungsten Hexamethoxides
Gulaim A. Seisenbaeva; Lars Kloo; Pia Werndrup; Vadim G. Kessler; Inorganic Chemistry 40 (2001) 3815–3818; doi:10.1021/ic0013173

data_4319977
_publ_section_title
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 Electrochemical Synthesis, X-ray Single Crystal, IR Spectroscopic, and
 Quantum Chemical Investigation of Molybdenum and Tungsten Hexamethoxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3815
_journal_page_last               3818
_journal_paper_doi               10.1021/ic0013173
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C6 H18 Mo O6'
_chemical_formula_weight         282.14
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 90.068(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.0976(13)
_cell_length_b                   6.6103(12)
_cell_length_c                   12.286(2)
_cell_measurement_reflns_used    999(I>10sigma(I))
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      3.08
_cell_volume                     576.43(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINTPLUS'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3208
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             288
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.0062(11)
_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   0.854
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0662
_reflns_number_gt                1011
_reflns_number_total             1302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0013173_1.cif
_cod_data_source_block           nimo2m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        576.41(18)
_cod_database_code               4319977