d(1) Oxosulfido-Mo(V) Compounds: First Isolation and Unambiguous Characterization of an Extended Series.
Doonan, Christian J.; Gourlay, Craig; Nielsen, David J.; Ng, Victor W. L.; Smith, Paul D.; Evans, David J.; George, Graham N.; White, Jonathan M.; Young, Charles G.; Inorganic chemistry 54 (2015) 6386–6396; doi:10.1021/acs.inorgchem.5b00708

data_4343248
_publ_section_title
;
 d(1) Oxosulfido-Mo(V) Compounds: First Isolation and Unambiguous
 Characterization of an Extended Series.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6386
_journal_page_last               6396
_journal_paper_doi               10.1021/acs.inorgchem.5b00708
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C30 H44 B Mo N7 O2, C2 H3 N'
_chemical_formula_sum            'C32 H47 B Mo N8 O2'
_chemical_formula_weight         682.53
_chemical_name_common            '[Tp(iPr)MoO(OC6H3Bu)(MeCN)].MeCN'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.05(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.446(3)
_cell_length_b                   12.235(2)
_cell_length_c                   23.269(5)
_cell_measurement_reflns_used    5135
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.96
_cell_measurement_theta_min      2.40
_cell_volume                     3489.0(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0926
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16018
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.413
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.8614
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_size_rad          0.2500
_refine_diff_density_max         3.481
_refine_diff_density_min         -3.036
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0953
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1707P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2289
_refine_ls_wR_factor_ref         0.2418
_reflns_number_gt                5829
_reflns_number_total             7400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00708_si_001.cif
_cod_data_source_block           decg21
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4343246--4343248.cif.
;
_cod_original_cell_volume        3489.1(12)
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               4343248
_exptl_absorpt_correction_t_ave  0.8615