A Kinetically Controlled Trans Bifunctionalized Organoimido Derivative of the Lindqvist-Type Hexamolybdate: Synthesis, Spectroscopic Characterization, and Crystal Structure of (n-Bu4N)2{trans-[Mo6O17(NAr)2]} (Ar = 2,6-dimethylphenyl)
Yun Xia; Yongge Wei; Yuan Wang; Hongyou Guo; Inorganic Chemistry 44 (2005) 9823–9828; doi:10.1021/ic051319t

data_4310249
_publ_section_title
;
A Kinetically Controlled Trans Bifunctionalized Organoimido Derivative of
the Lindqvist-Type Hexamolybdate: Synthesis, Spectroscopic
Characterization, and Crystal Structure of (n-Bu4N)2{trans-[Mo6O17(NAr)2]}
(Ar = 2,6-dimethylphenyl)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9823
_journal_page_last               9828
_journal_paper_doi               10.1021/ic051319t
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C48 H90 Mo6 N4 O17'
_chemical_formula_weight         1570.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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                 105.377(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.0358(17)
_cell_length_b                   16.569(3)
_cell_length_c                   17.507(3)
_cell_measurement_reflns_used    7535
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      2.3248
_cell_volume                     3086.6(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23152
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_T_max  0.6694
_exptl_absorpt_correction_T_min  0.3687
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.233
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         7036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+2.3811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0900
_reflns_number_gt                6257
_reflns_number_total             7036
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051319tsi20050803_063026.cif
_cod_data_source_block           test
_cod_original_cell_volume        3086.5(8)
_cod_database_code               4310249