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_4317730
_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_structural     'Mo2 (O2C16H23)4BF4, 2CH2Cl2'
_chemical_formula_sum            'C66 H96 B Cl4 F4 Mo2 O8'
_chemical_formula_weight         1437.92
_chemical_melting_point          ?
_chemical_name_systematic
;
tetrakis(m^2-2,4,6-triisopropylbenzoato-O, O') molybdenum (II,III)
tetrafluoroborate, dichloromethane solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.210(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.2621(7)
_cell_length_b                   18.7552(13)
_cell_length_c                   20.5100(15)
_cell_measurement_reflns_used    5034
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.4875
_cell_measurement_theta_min      2.277
_cell_volume                     3526.3(4)
_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  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17073
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.01
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.95983
_exptl_absorpt_correction_T_min  0.75020
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1498
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.109
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.927
_refine_ls_goodness_of_fit_obs   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5467
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      0.942
_refine_ls_restrained_S_obs      1.024
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_obs          0.0500
_refine_ls_shift/esd_max         -2.253
_refine_ls_shift/esd_mean        0.080
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+8.3976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1438
_refine_ls_wR_factor_obs         0.1248
_reflns_number_observed          3622
_reflns_number_total             5538
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic011079r_2.cif
_cod_data_source_block           compound2
_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^)+(0.0774P)^2^+8.3976P] 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^)+(0.0774P)^2^+8.3976P] 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               4317730