Bis[bis(triphenylphosphine)iminium] Hexamolybdate
Hoppe, S.; Stark, J. L.; Whitmire, K. H.; Acta Crystallographica Section C 53 (1997) 68–70; doi:10.1107/S0108270196011791

data_2005851
_publ_section_title
;
 Bis[bis(triphenylphosphine)iminium] Hexamolybdate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              68
_journal_page_last               70
_journal_paper_doi               10.1107/S0108270196011791
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '(C36 H30 N P2)2 [Mo6 O19]'
_chemical_formula_moiety         '(C36 H30 N P2 +)2 (Mo6 O19 2-)'
_chemical_formula_structural
;
((((C6H5)3) P)2 N)2 (Mo6O19)
;
_chemical_formula_sum            'C72 H60 Mo6 N2 O19 P4'
_chemical_formula_weight         1956.74
_chemical_melting_point          545.15
_chemical_name_systematic
;
 Bis (bistriphenylphosphineimine) hexamolybdate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                61.62(3)
_cell_angle_beta                 84.55(3)
_cell_angle_gamma                87.83(3)
_cell_formula_units_Z            1
_cell_length_a                   11.368(2)
_cell_length_b                   13.490(3)
_cell_length_c                   13.573(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      9.84
_cell_measurement_theta_min      3.72
_cell_volume                     1823.0(8)
_computing_cell_refinement       TEXSAN
_computing_data_collection
'TEXSAN (Molecular Structure Corporation, 1990)'
_computing_data_reduction        TEXSAN
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1992)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5300
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.161
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_description       block
_exptl_crystal_F_000             970
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.730
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.046
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_hydrogen_treatment
'H-atom parameters calculated, riding model refinement, fixed U~iso~'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         5026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_restrained_S_obs      1.078
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_obs          0.0471
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.6372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1228
_refine_ls_wR_factor_obs         0.1086
_reflns_number_observed          3804
_reflns_number_total             5026
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bs1007.cif
_cod_data_source_block           hexa
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '272_C' was changed to '545.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.6372P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.6372P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1823.0(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2005851