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_7028226
_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         'C7 H18 N, Cl H2 Mo O6 '
_chemical_formula_sum            'C7 H20 Cl Mo N O6'
_chemical_formula_weight         345.63
_chemical_name_common
;
Triethylammonium aquachlorooxodiperoxomolybdate
;
_chemical_name_systematic
; 
Triethylmethylammonium 
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            4
_cell_length_a                   8.219(4)
_cell_length_b                   11.656(5)
_cell_length_c                   13.671(6)
_cell_measurement_reflns_used    5170
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      30.0348
_cell_measurement_theta_min      2.8918
_cell_volume                     1309.7(10)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12139
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    1.217
_exptl_absorpt_correction_T_max  0.9706
_exptl_absorpt_correction_T_min  0.8628
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.233
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0275P)^2^+1.7499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0704
_reflns_number_gt                3561
_reflns_number_total             3821
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52848k.txt
_cod_data_source_block           g:\sx97n\Et3MeN-MoCl
_cod_database_code               7028226