Synthesis and Characterization of Unsymmetrical (cis-(Phosphino-arsino)ethene)tetracarbonylmolybdenum Complexes: Hydroarsination Reactions of (H3CC\τbCPPh2)Mo(CO)5 and [H2CCCH(DBP)]Mo(CO)5 and Hydrophosphination Reactions of (Ph2AsCH2C\τbCH)Mo(CO)5
Kalyani Maitra; Vincent J. Catalano; Jerry Clark; John H. Nelson; Inorganic Chemistry 37 (1998) 1105–1111; doi:10.1021/ic9711170

data_4322683
_publ_section_title
;
 Synthesis and Characterization of Unsymmetrical
 (cis-(Phosphino-arsino)ethene)tetracarbonylmolybdenum Complexes:
 Hydroarsination Reactions of (H3CC\\tbCPPh2)Mo(CO)5 and
 [H2CCCH(DBP)]Mo(CO)5 and Hydrophosphination Reactions of
 (Ph2AsCH2C\\tbCH)Mo(CO)5
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1105
_journal_page_last               1111
_journal_paper_doi               10.1021/ic9711170
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C20 H13 As Mo O5'
_chemical_formula_weight         504.16
_chemical_name_common            G
_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                 95.191(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.848(2)
_cell_length_b                   13.006(3)
_cell_length_c                   13.506(2)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.51
_cell_measurement_theta_min      4.65
_cell_volume                     2072.7(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_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      298(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
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4606
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        4.78
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.243
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3902
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
_exptl_crystal_size_max          .02
_exptl_crystal_size_mid          .04
_exptl_crystal_size_min          .11
_refine_diff_density_max         0.785
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       0.0031(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.030
_refine_ls_goodness_of_fit_obs   1.094
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_restrained_S_obs      1.094
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_obs          0.0673
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1257P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1942
_refine_ls_wR_factor_obs         0.1691
_reflns_number_observed          2595
_reflns_number_total             3637
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9711170_3.cif
_cod_data_source_block           vjc157
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1257P)^2^+0.0000P] 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^)+(0.1257P)^2^+0.0000P] 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_database_code               4322683