A new aqueous molybdenum cluster with a Mo~3~(u~3~-CCH~3~)(μ~3~-O) trinuclear core
Kris A. Pineda; James C. Fettinger; Jacqueline R. Houston; Inorganica Chimica Acta 392 (2012) 485–489; doi:10.1016/j.ica.2012.03.037

data_1512663
_publ_section_title
;
 A new aqueous molybdenum cluster with a Mo~3~(u~3~-CCH~3~)(\m~3~-O)
 trinuclear core
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              485
_journal_page_last               489
_journal_paper_doi               10.1016/j.ica.2012.03.037
_journal_volume                  392
_journal_year                    2012
_chemical_formula_moiety         'C41 H80 Mo6 O32, 8(H2 O), 2(Br)'
_chemical_formula_sum            'C41 H96 Br2 Mo6 O40'
_chemical_formula_weight         1964.64
_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
_cell_angle_alpha                60.0511(12)
_cell_angle_beta                 88.9275(12)
_cell_angle_gamma                70.2585(13)
_cell_formula_units_Z            1
_cell_length_a                   11.6658(11)
_cell_length_b                   13.7602(12)
_cell_length_c                   13.7673(12)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.28
_cell_volume                     1771.6(3)
_computing_cell_refinement       'SAINT (7.68A) (Bruker, 2009)'
_computing_data_collection       'SMART (Version 5.054) (Bruker, 2002)'
_computing_data_reduction        'SAINT (7.68A) (Bruker, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28851
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    2.248
_exptl_absorpt_correction_T_max  0.8549
_exptl_absorpt_correction_T_min  0.6984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            Red-Orange
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         8131
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0162P)^2^+2.1689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0555
_reflns_number_gt                6953
_reflns_number_total             8131
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012-392-485-489.cif
_cod_data_source_block           jf2069f2
_cod_database_code               1512663