A novel dinuclear Mo^VI^ complex with tris(3,5-dimethyl-1<i>H</i>-pyrazol-1-yl)methane
Gago, Sandra; Gomes, Ana C.; Cunha-Silva, Luís; Pillinger, Martyn; Gonçalves, Isabel S.; Almeida Paz, Filipe A.; Acta Crystallographica Section C 68 (2012) m73–m75; doi:10.1107/S0108270112004507

data_2018425
_publ_section_title
;
 A novel dinuclear Mo^VI^ complex with
 tris(3,5-dimethyl-1<i>H</i>-pyrazol-1-yl)methane
;
_journal_coeditor_code           SK3427
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m73
_journal_page_last               m75
_journal_paper_doi               10.1107/S0108270112004507
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Mo2 Cl2 O4 (C16 H22 N6)], C2 H3 N'
_chemical_formula_moiety         'C16 H22 Cl2 Mo2 N6 O5, C2 H3 N'
_chemical_formula_sum            'C18 H25 Cl2 Mo2 N7 O5'
_chemical_formula_weight         682.23
_chemical_name_systematic
;
dichlorido-2\k^2^<i>Cl</i>-\m-oxido-\k^2^<i>O</i>:<i>O</i>-tetraoxido-
1\k^2^<i>O</i>,2\k^2^<i>O</i>-[tris(3,5-dimethyl-1<i>H</i>-pyrazol-1-yl-
1\k<i>N</i>^2^)methane]dimolybdenum(IV) acetonitrile monosolvate
;
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6346(5)
_cell_length_b                   21.6152(12)
_cell_length_c                   13.6021(8)
_cell_measurement_reflns_used    9084
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.24
_cell_measurement_theta_min      2.54
_cell_volume                     2538.7(3)
_computing_cell_refinement       'APEX2 (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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII X8 KappaCCD area-detector'
_diffrn_measurement_method       '\w and \f'
_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  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            59602
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         3.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.241
_exptl_absorpt_correction_T_max  0.9292
_exptl_absorpt_correction_T_min  0.8755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.886
_refine_diff_density_min         -1.533
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0721P)^2^+2.6754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                3061
_reflns_number_total             3526
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3427.cif
_cod_data_source_block           I
_cod_database_code               2018425
_cod_database_fobs_code          2018425