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_4117139
_publ_section_title
;
 Stable Mononuclear, 17-Electron Molybdenum(III) Carbonyl Complexes.
 Synthesis, Structure, Thermal Decomposition, and Cl-Addition Reactions
;
_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            'C41 H47 Cl F6 Mo O2 P3'
_chemical_formula_weight         910.09
_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                 99.119(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7394(14)
_cell_length_b                   20.421(2)
_cell_length_c                   14.8567(15)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      39.2
_cell_measurement_theta_min      33.5
_cell_volume                     4115.7(7)
_computing_cell_refinement       'Enraf EXPRESS'
_computing_data_collection       'Enraf EXPRESS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'NRCVAX ORTEP'
_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       'Enraf CAD4'
_diffrn_measurement_method       '\w/2t\ 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  0.0572
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_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5628
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  0.5577
_exptl_absorpt_correction_T_min  0.2938
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            reddish-orange
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       plate
_exptl_crystal_F_000             1868
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.114
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_refine_ls_number_reflns         5366
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_refine_ls_restrained_S_obs      1.066
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_refine_ls_R_factor_obs          0.0459
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+8.4227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1211
_refine_ls_wR_factor_obs         0.1077
_reflns_number_observed          4299
_reflns_number_total             5367
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9540738_1.cif
_cod_data_source_block           e
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+8.4227P] 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^)+(0.0643P)^2^+8.4227P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        4115.8(8)
_cod_database_code               4117139