Filling a Void: Isolation and Characterization of Tetracarboxylato Dimolybdenum Cations
F. Albert Cotton; Lee M. Daniels; Elizabeth A. Hillard; Carlos A. Murillo; Inorganic Chemistry 41 (2002) 1639–1644; doi:10.1021/ic011079r

data_4317732
_publ_section_title
;
 Filling a Void: Isolation and Characterization of Tetracarboxylato
 Dimolybdenum Cations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1639
_journal_page_last               1644
_journal_paper_doi               10.1021/ic011079r
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'C20 H36 F6 Mo2 O8 P'
_chemical_formula_structural     'Mo2 (O2C5H9)4 PF6'
_chemical_formula_sum            'C20 H36 F6 Mo2 O8 P'
_chemical_formula_weight         741.34
_chemical_melting_point          ?
_chemical_name_systematic
;
 tetrakis(m^2-pivalato-O, O') molybdenum (II, III) hexaflurophosphate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 115.351(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.764(4)
_cell_length_b                   10.454(2)
_cell_length_c                   19.246(4)
_cell_measurement_reflns_used    6400
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.488
_cell_measurement_theta_min      2.342
_cell_volume                     3048.1(11)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Bruker SMART area detector'
_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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9279
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.37
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.429
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.175
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.094
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3486
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.091
_refine_ls_restrained_S_obs      1.088
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_obs          0.0277
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+3.6777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0765
_refine_ls_wR_factor_obs         0.0716
_reflns_number_observed          3090
_reflns_number_total             3486
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic011079r_4.cif
_cod_data_source_block           compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+3.6777P] 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^)+(0.0357P)^2^+3.6777P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4317732