Stable Mononuclear, 17-Electron Molybdenum(III) Carbonyl Complexes. Synthesis, Structure, Thermal Decomposition, and Cl-Addition Reactions
James C. Fettinger; D. Webster Keogh; Rinaldo Poli; Journal of the American Chemical Society 118 (1996) 3617–3625; doi:10.1021/ja9540738

data_4117140
_publ_section_title
;
 Stable Mononuclear, 17-Electron Molybdenum(III) Carbonyl Complexes.
 Synthesis, Structure, Thermal Decomposition, and Cl-Addition Reactions
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3617
_journal_page_last               3625
_journal_paper_doi               10.1021/ja9540738
_journal_volume                  118
_journal_year                    1996
_chemical_formula_sum            'C35 H35 Cl F7 Mo N2 P3'
_chemical_formula_weight         840.95
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.225(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.160(2)
_cell_length_b                   10.942(2)
_cell_length_c                   25.010(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      11.9
_cell_volume                     3586.4(10)
_computing_cell_refinement       'Enraf EXPRESS 5.0'
_computing_data_collection       'Enraf EXPRESS 5.0'
_computing_data_reduction        'Harms XCAD4'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_sigmaI/netI    0.0109
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_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
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_diffrn_reflns_limit_l_min       -32
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_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            reddish-orange
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_goodness_of_fit_obs   1.115
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_refine_ls_restrained_S_obs      1.115
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_obs          0.0411
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_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+9.7624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1198
_refine_ls_wR_factor_obs         0.1181
_reflns_number_observed          5964
_reflns_number_total             6310
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9540738_2.cif
_cod_data_source_block           q
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+9.7624P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+9.7624P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3586.4(9)
_cod_database_code               4117140