Bis[tris(2-ammonioethyl)amine] bis(pentafluoridooxidomolybdate) difluoride monohydrate
K. Adil; J. Marrot; M. Leblanc; V. Maisonneuve; Acta Crystallographica Section E 63 (2007) m1511–m1513; doi:10.1107/S1600536807018077

data_2213268
_publ_section_title
;
 Bis[tris(2-ammonioethyl)amine] bis(pentafluoridooxidomolybdate)
 difluoride monohydrate
;
_journal_coeditor_code           DN2118
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1511
_journal_page_last               m1513
_journal_paper_doi               10.1107/S1600536807018077
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C6 H21 N4)2 '[Mo F5 O]2 F2, H2 O''
_chemical_formula_moiety
'2(C6 H21 N4 3+), 2(F5 Mo O 2-), 2(F -), H2 O'
_chemical_formula_sum            'C12 H44 F12 Mo2 N8 O3'
_chemical_formula_weight         768.39
_chemical_name_common            '[N(CH2CH2NH3)3]2.(MoOF5)2.(F)2.H2O'
_chemical_name_systematic
;
Bis[tris(2-ammonioethyl)amine] bis(pentafluoridooxidomolybdate) difluoride
monohydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 100.939(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9666(8)
_cell_length_b                   11.3068(6)
_cell_length_c                   19.7260(13)
_cell_measurement_reflns_used    31578
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      2
_cell_volume                     2839.5(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'ENCIFER (Allen <i>et al.</i>,  2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.1118
_diffrn_reflns_av_sigmaI/netI    0.0926
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30643
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.94
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'parallepiped '
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.669
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3260
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+6.658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1111
_reflns_number_gt                2225
_reflns_number_total             4103
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn2118.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2213268
_cod_database_fobs_code          2213268