Synthesis, structure and spectroscopic analyses of aquachloridooxidodiperoxidomolybdate(VI).
Saito, Masa-aki; Hashimoto, Masato; Dalton transactions (Cambridge, England : 2003) 43 (2014) 402–405; doi:10.1039/c3dt52848k

data_7028225
_publ_section_title
;
 Synthesis, structure and spectroscopic analyses of
 aquachloridooxidodiperoxidomolybdate(VI).
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              402
_journal_page_last               405
_journal_paper_doi               10.1039/c3dt52848k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C8 H20 N, Cl H2 Mo O6 '
_chemical_formula_sum            'C8 H22 Cl Mo N O6'
_chemical_formula_weight         359.66
_chemical_name_common
;
Tetraethylammonium aquachlorooxodiperoxomolybdate(VI)
;
_chemical_name_systematic
; 
 Tetraethylammonium
 Aquachloridooxidodi(peroxido-\k^2^O,O)molybdate(VI) 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.9240(11)
_cell_length_b                   11.5240(17)
_cell_length_c                   31.625(4)
_cell_measurement_reflns_used    10377
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      30.0441
_cell_measurement_theta_min      2.6187
_cell_volume                     2887.9(7)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'ORTEP-III for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'RIGAKU SATURN724+ (4x4 bin mode)'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            26411
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  0.9621
_exptl_absorpt_correction_T_min  0.9044
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.054
_refine_diff_density_max         1.028
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         8417
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0275P)^2^+1.2956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0644
_reflns_number_gt                7864
_reflns_number_total             8417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52848k.txt
_cod_data_source_block           g:\sx97n\Et4N-MoCl
_cod_database_code               7028225