μ-Oxido-bis[chlorido(4,4'-di-<i>tert</i>-butyl-2,2'-bipyridine-κ^2^<i>N</i>,<i>N</i>')dioxidomolybdenum(VI)] 0.2-hydrate
Gomes, Ana C.; Fernandes, José A.; Gamelas, Carla A.; Gonçalves, Isabel S.; Almeida Paz, Filipe A.; Acta Crystallographica Section E 67 (2011) m1738–m1739; doi:10.1107/S1600536811046952

data_2232964
_publ_section_title
;
 \m-Oxido-bis[chlorido(4,4'-di-<i>tert</i>-butyl-2,2'-bipyridine-\k^2^<i>N</i>,<i>N</i>')dioxidomolybdenum(VI)]
 0.2-hydrate
;
_journal_coeditor_code           TK5013
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1738
_journal_page_last               m1739
_journal_paper_doi               10.1107/S1600536811046952
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Mo2 Cl2 O5 (C18 H24 N2)2], 0.2H2 O'
_chemical_formula_moiety         'C36 H48 Cl2 Mo2 N4 O5, 0.2(H2 O)'
_chemical_formula_sum            'C36 H48.4 Cl2 Mo2 N4 O5.2'
_chemical_formula_weight         883.17
_chemical_name_systematic
;
\m-Oxido-bis[chlorido(4,4'-di-<i>tert</i>-butyl-2,2'-bipyridine-
\k^2^<i>N</i>,<i>N</i>')dioxidomolybdenum(VI)] 0.2-hydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 99.582(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9997(7)
_cell_length_b                   12.7444(6)
_cell_length_c                   18.4609(8)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.08
_cell_measurement_theta_min      2.75
_cell_volume                     3943.8(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            54239
_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    0.816
_exptl_absorpt_correction_T_max  0.9759
_exptl_absorpt_correction_T_min  0.9376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1997)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.960
_refine_diff_density_min         -0.666
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         10578
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0315P)^2^+3.4060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                7469
_reflns_number_total             10578
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk5013.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C36 H48.40 Cl2 Mo2 N4 O5.20'
_cod_database_code               2232964
_cod_database_fobs_code          2232964