A new mono-functionalized organoimido hexamolybdate derivative: bis(tetra-<i>n</i>-butylammonium) (5-chloro-2-methylphenylimido)-μ~6~-oxido-dodeca-μ~2~-oxido-pentaoxidohexamolybdate(VI)
Li, Qiang; Xiao, Zichen; Chen, Liye; Zhang, Jin; Acta Crystallographica Section E 67 (2011) m1404–m1405; doi:10.1107/S1600536811036063

data_2231804
_publ_section_title
;
 A new mono-functionalized organoimido hexamolybdate derivative:
 bis(tetra-<i>n</i>-butylammonium)
 (5-chloro-2-methylphenylimido)-\m~6~-oxido-dodeca-\m~2~-oxido-pentaoxidohexamolybdate(VI)
;
_journal_coeditor_code           BH2377
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1404
_journal_page_last               m1405
_journal_paper_doi               10.1107/S1600536811036063
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C16 H36 N)2 [Mo6 (C7 H6 Cl N) O18]'
_chemical_formula_moiety         '2(C16 H36 N +), C7 H6 Cl Mo6 N O18 2-'
_chemical_formula_sum            'C39 H78 Cl Mo6 N3 O18'
_chemical_formula_weight         1488.13
_chemical_name_systematic
;
bis(tetra-<i>n</i>-butylammonium) (5-chloro-2-methylphenylimido)-
\m~6~-oxido-dodeca-\m~2~-oxido-pentaoxidohexamolybdate(VI)
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 94.0770(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9184(9)
_cell_length_b                   20.7309(16)
_cell_length_c                   20.6731(15)
_cell_measurement_reflns_used    6101
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      24.65
_cell_measurement_theta_min      2.20
_cell_volume                     5522.5(7)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruke SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w 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  0.0708
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33748
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_T_max  0.8698
_exptl_absorpt_correction_T_min  0.6727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.505
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     604
_refine_ls_number_reflns         10841
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0498P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1184
_reflns_number_gt                6533
_reflns_number_total             10841
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh2377.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-P 2ybc'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2231804
_cod_database_fobs_code          2231804