Oxalate Bridged Triangles Incorporating Mo24+ Units. Electronic Structure and Bonding
Malcolm H. Chisholm; Nathan J. Patmore; Carly R. Reed; Namrata Singh; Inorganic Chemistry 49 (2010) 7116–7122; doi:10.1021/ic1009237

data_4316161
_publ_section_title
;
 Oxalate Bridged Triangles Incorporating Mo24+ Units. Electronic Structure
 and Bonding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7116
_journal_page_last               7122
_journal_paper_doi               10.1021/ic1009237
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C96 H87 Mo6 N12 O24, 7(C6 H4 Cl2)'
_chemical_formula_sum            'C138 H108 Cl14 Mo6 N12 O24'
_chemical_formula_weight         3390.30
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 103.617(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.7412(6)
_cell_length_b                   25.6515(9)
_cell_length_c                   32.0808(12)
_cell_measurement_reflns_used    8107
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.1775
_cell_measurement_theta_min      2.5035
_cell_volume                     13389.4(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            143133
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.03
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_T_max  0.9396
_exptl_absorpt_correction_T_min  0.8692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             6808
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_platon_squeeze_details
; 
The unit cell contains an additional 20 1,2-dichloromethane 
molecules which have been treated as a diffuse contribution to
the overall scattering without specific atom positions by
SQUEEZE/PLATON.
;
_refine_diff_density_max         1.661
_refine_diff_density_min         -1.363
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1283
_refine_ls_number_reflns         23563
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1374P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2164
_refine_ls_wR_factor_ref         0.2368
_reflns_number_gt                13100
_reflns_number_total             23563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1009237_si_002.cif
_cod_data_source_block           ComplexII
_cod_original_sg_symbol_Hall     '-p 2ybc'
_cod_database_code               4316161