Bis(tetrabutylammonium) [2-(ethoxycarbony)phenylimido]-μ~6~-oxido-dodeca-μ~2~-oxido-pentaoxidohexamolybdenum diethyl ether hemisolvate
Wang, Manxiang; Tao, Shikai; Guo, Jing; Hao, Jian; Li, Qiang; Acta Crystallographica Section E 68 (2012) m926–m927; doi:10.1107/S1600536812026323

data_2235349
_publ_section_title
;
 Bis(tetrabutylammonium)
 [2-(ethoxycarbony)phenylimido]-\m~6~-oxido-dodeca-\m~2~-oxido-pentaoxidohexamolybdenum
 diethyl ether hemisolvate
;
_journal_coeditor_code           BH2428
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m926
_journal_page_last               m927
_journal_paper_doi               10.1107/S1600536812026323
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'(C16 H36 N)2 [Mo6 O18 (C9 H9 N O2)], 0.5C4 H10 O'
_chemical_formula_moiety
'2(C16 H36 N +), C9 H9 Mo6 N O20 2-, 0.5(C4 H10 O)'
_chemical_formula_sum            'C43 H86 Mo6 N3 O20.5'
_chemical_formula_weight         1548.79
_chemical_name_systematic
;
Bis(tetrabutylammonium)
[2-(ethoxycarbony)phenylimido]-\m~6~-oxido-dodeca-\m~2~-oxido-
pentaoxidohexamolybdenum diethyl ether hemisolvate
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.709(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3974(16)
_cell_length_b                   17.0854(8)
_cell_length_c                   21.687(3)
_cell_measurement_reflns_used    9126
_cell_measurement_temperature    101
_cell_measurement_theta_max      29.2571
_cell_measurement_theta_min      3.0042
_cell_volume                     5819.2(11)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2010)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      101
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Agilent Xcalibur Eos Gemini'
_diffrn_measurement_method       '\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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31709
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    1.325
_exptl_absorpt_correction_T_max  0.7330
_exptl_absorpt_correction_T_min  0.6193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2011)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3124
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.462
_refine_diff_density_min         -0.805
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     854
_refine_ls_number_reflns         11422
_refine_ls_number_restraints     500
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+15.7229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                8774
_reflns_number_total             11422
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh2428.cif
_cod_data_source_block           I
_cod_original_cell_volume        5819.1(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C43 H86 Mo6 N3 O20.50'
_cod_database_code               2235349
_cod_database_fobs_code          2235349