Tris(4,4'-di-<i>tert</i>-butyl-2,2'-bipyridine-κ^2^<i>N</i>,<i>N</i>')molybdenum(II) μ~6~-oxido-dodeca-μ~2~-oxido-hexaoxidohexamolybdate(VI) acetonitrile tetrasolvate
Amarante, Tatiana R.; Fernandes, José A.; Gonçalves, Isabel S.; Almeida Paz, Filipe A.; Acta Crystallographica Section E 67 (2011) m1828–m1829; doi:10.1107/S1600536811049385

data_2232970
_publ_section_title
;
 Tris(4,4'-di-<i>tert</i>-butyl-2,2'-bipyridine-\k^2^<i>N</i>,<i>N</i>')molybdenum(II)
 \m~6~-oxido-dodeca-\m~2~-oxido-hexaoxidohexamolybdate(VI) acetonitrile
 tetrasolvate
;
_journal_coeditor_code           TK5024
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1828
_journal_page_last               m1829
_journal_paper_doi               10.1107/S1600536811049385
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Mo (C18 H24 N2)3] [Mo6 O19], 4C2 H3 N'
_chemical_formula_moiety         'C54 H72 Mo N6 2+, Mo6 O19 2-, 4(C2 H3 N)'
_chemical_formula_sum            'C62 H84 Mo7 N10 O19'
_chemical_formula_weight         1944.97
_chemical_name_systematic
;
Tris(4,4'-di-<i>tert</i>-butyl-2,2'-bipyridine-
\k^2^<i>N</i>,<i>N</i>')molybdenum(II)
\m~6~-oxido-dodeca-\m~2~-oxido-hexaoxidohexamolybdate(VI) acetonitrile
tetrasolvate
;
_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                90.144(3)
_cell_angle_beta                 103.862(2)
_cell_angle_gamma                107.547(2)
_cell_formula_units_Z            2
_cell_length_a                   14.4202(8)
_cell_length_b                   16.3205(9)
_cell_length_c                   17.1122(10)
_cell_measurement_reflns_used    9781
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.87
_cell_measurement_theta_min      2.46
_cell_volume                     3715.9(4)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker X8 KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f 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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            209835
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.215
_exptl_absorpt_correction_T_max  0.9090
_exptl_absorpt_correction_T_min  0.8200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1997)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.294
_refine_diff_density_min         -3.956
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     970
_refine_ls_number_reflns         22527
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0699P)^2^+12.1066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1486
_reflns_number_gt                17706
_reflns_number_total             22527
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk5024.cif
_cod_data_source_block           I
_cod_database_code               2232970
_cod_database_fobs_code          2232970