Crystal structure of (2,2'-bi-pyridine-κ<sup>2</sup><i>N</i>,<i>N</i>')-<i>trans</i>-bis-(<i>tert</i>-butyl-dimethyl-sil-yloxy)-<i>cis</i>-dioxidomolybdenum(VI).
Minyaev, Mikhail E.; Vinogradov, Alexander A.; Nifant'ev, Ilya E.; Churakov, Andrei V.; Acta crystallographica. Section E, Crystallographic communications 74 (2018) 970–972; doi:10.1107/S2056989018008472

data_2312114
_publ_section_title
;
 Crystal structure of
 (2,2'-bi-pyridine-&#x3ba;<sup>2</sup><i>N</i>,<i>N</i>')-<i>trans</i>-bis-(<i>tert</i>-butyl-dimethyl-sil-yloxy)-<i>cis</i>-dioxidomolybdenum(VI).
;
_journal_issue                   'Pt 7'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              970
_journal_page_last               972
_journal_paper_doi               10.1107/S2056989018008472
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Mo (C6 H15 O Si)2 O2 (C10 H8 N2)]'
_chemical_formula_moiety         'C22 H38 Mo N2 O4 Si2'
_chemical_formula_sum            'C22 H38 Mo N2 O4 Si2'
_chemical_formula_weight         546.66
_chemical_name_common
;
Bis(tert-butyldimethylsilyloxy)dioxomolybdenum(2,2'-bipyridyl)
;
_chemical_name_systematic
;
(2,2'-Bipyridine-\k^2^<i>N</i>,<i>N</i>')-<i>trans</i>-bis(<i>tert</i>-\
butyldimethylsilyloxy)-<i>cis</i>-dioxiomolybdenum(VI)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                113.144(2)
_cell_angle_beta                 91.133(2)
_cell_angle_gamma                105.501(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4027(8)
_cell_length_b                   12.8657(13)
_cell_length_c                   14.4266(14)
_cell_measurement_reflns_used    4261
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.155
_cell_measurement_theta_min      2.541
_cell_volume                     1368.1(2)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
<i>SHELXL2017/1</i> (Sheldrick, 2015) and publCIF (Westrip,
2010)
;
_computing_structure_refinement
;
<i>SHELXL2017/1</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       \w
_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  0.0300
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14073
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         2.541
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.7971
_exptl_absorpt_correction_T_min  0.6122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.757
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         6550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+0.2626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0747
_reflns_number_gt                5158
_reflns_number_total             6550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5447sup1.cif
_cod_data_source_block           I
_cod_database_code               2312114
_shelx_estimated_absorpt_t_min   0.810
_shelx_estimated_absorpt_t_max   0.994
_shelx_hkl_checksum              41661
_shelx_res_checksum              88730
_cod_database_fobs_code 2312114