Convenient syntheses and structural characterizations of mono-substituted alkylimido hexamolybdates: [Mo6O18(NR)]2− (R = Me, Et, n-Pr, i-Pr, n-Bu, t-Bu, Cy, Hex, Ode)
Li, Qiang; Wang, Longsheng; Yin, Panchao; Wei, Yongge; Hao, Jian; Zhu, Yulin; Zhu, Li; Yuan, Gu; Dalton Transactions  (2009) 1172–1179; doi:10.1039/b813924e

data_7000463
_publ_section_title
;
 Convenient syntheses and structural characterizations of
 mono-substituted alkylimido hexamolybdates: [Mo6O18(NR)]2&#x2212; (R =
 Me, Et, n-Pr, i-Pr, n-Bu, t-Bu, Cy, Hex, Ode)
;
_journal_coden_ASTM              DTARAF
_journal_issue                   7
_journal_name_full               'Dalton Transactions'
_journal_page_first              1172
_journal_page_last               1179
_journal_paper_doi               10.1039/b813924e
_journal_year                    2009
_chemical_formula_sum            'C38 H83 Mo6 N3 O18'
_chemical_formula_weight         1445.71
_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                93.7700(10)
_cell_angle_beta                 103.1410(10)
_cell_angle_gamma                91.4990(10)
_cell_formula_units_Z            4
_cell_length_a                   12.5288(4)
_cell_length_b                   19.4569(6)
_cell_length_c                   23.1302(7)
_cell_measurement_reflns_used    5741
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.72
_cell_volume                     5474.0(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44067
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.398
_exptl_absorpt_correction_T_max  0.7970
_exptl_absorpt_correction_T_min  0.5656
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.677
_refine_diff_density_min         -1.960
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1141
_refine_ls_number_reflns         18581
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.418
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+21.3101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1489
_reflns_number_gt                12438
_reflns_number_total             18581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B813924e.txt
_cod_data_source_block           compound-7I
_cod_database_code               7000463