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_4317731
_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_formula_moiety         'C64 H92 Mo2 O8'
_chemical_formula_sum            'C64 H92 Mo2 O8'
_chemical_formula_weight         1181.26
_chemical_melting_point          ?
_chemical_name_systematic
;
 tetrakis(m^2-2,4,6-triisopropylbenzoato-O, O') dimolybdenum (II,II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.01(4)
_cell_angle_beta                 107.95(3)
_cell_angle_gamma                103.36(6)
_cell_formula_units_Z            1
_cell_length_a                   9.709(6)
_cell_length_b                   12.035(8)
_cell_length_c                   14.574(6)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.1
_cell_volume                     1520.0(17)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        XPREP
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Nonius FAST'
_diffrn_measurement_method       'Ellipsoid mask-fitting'
_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  0.0745
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7961
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         2.26
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.464
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.450
_refine_diff_density_min         -1.588
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         3996
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.832
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1648
_reflns_number_gt                3651
_reflns_number_total             3996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011079r_3.cif
_cod_data_source_block           compound3
_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 
;
_cod_original_cell_volume        1520.0(15)
_cod_database_code               4317731