Syntheses, Reactivity, and Crystal Structures of Molybdenum Complexes with Pyridine-2-thionate (pyS)-Containing Ligands: Crystal Structures of [Mo(η3-C3H5)(CO)2]2(μ-η1,η2-pyS)2, exo-[Mo(η3-C3H5)(CO)(η2-pyS)(η2-dppe)], [Mo(CO)3(η1-SC5H4NH)(η2-dppm)], and [Mo(CO)(η2-pyS)2(η2-dppm)]
Kuang-Hway Yih; Gene-Hsiang Lee; Yu Wang; Inorganic Chemistry 42 (2003) 1092–1100; doi:10.1021/ic020579x

data_4313121
_publ_section_title
;
 Syntheses, Reactivity, and Crystal Structures of Molybdenum Complexes
 with Pyridine-2-thionate (pyS)-Containing Ligands: Crystal Structures of
 [Mo(\h3-C3H5)(CO)2]2(\m-\h1,\h2-pyS)2,
 exo-[Mo(\h3-C3H5)(CO)(\h2-pyS)(\h2-dppe)],
 [Mo(CO)3(\h1-SC5H4NH)(\h2-dppm)], and [Mo(CO)(\h2-pyS)2(\h2-dppm)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1092
_journal_page_last               1100
_journal_paper_doi               10.1021/ic020579x
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C30 H25 Mo N O3 P2'
_chemical_formula_weight         605.39
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
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_symmetry_space_group_name_Hall  '-P 2ybc'
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_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                 109.07(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.930(2)
_cell_length_b                   18.516(4)
_cell_length_c                   15.173(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
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_cell_measurement_theta_min      9.37
_cell_volume                     2902.2(11)
_computing_cell_refinement       'NONIUS CAD4'
_computing_data_collection       'NONIUS CAD4'
_computing_data_reduction        NRCSDP
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'NONIUS CAD4'
_diffrn_measurement_method       '\w-2\q 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1409
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
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_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3772
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  0.8907
_exptl_absorpt_correction_T_min  0.8423
_exptl_absorpt_correction_type   ' empirical used psi-scan'
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
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_exptl_crystal_size_min          0.20
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_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.1301
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0124P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0902
_reflns_number_gt                1888
_reflns_number_total             3772
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020579x_1.cif
_cod_data_source_block           ic3170
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2902.1(10)
_cod_database_code               4313121