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_4322681
_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            'C31 H24 As Mo O4 P'
_chemical_formula_weight         662.33
_chemical_name_common            E
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.192(2)
_cell_length_b                   21.649(4)
_cell_length_c                   7.7420(10)
_cell_measurement_reflns_used    49
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.41
_cell_measurement_theta_min      1.88
_cell_volume                     2881.5(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      293(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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0653
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3392
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.88
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.684
_exptl_absorpt_correction_T_max  0.8169
_exptl_absorpt_correction_T_min  0.7466
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            light_orange
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       oblate
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .6
_exptl_crystal_size_min          .4
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.156
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_restrained_S_obs      1.156
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_obs          0.0544
_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^)+(0.0648P)^2^+2.8010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1432
_refine_ls_wR_factor_obs         0.1215
_reflns_number_observed          1611
_reflns_number_total             2593
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9711170_1.cif
_cod_data_source_block           jhn016c
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+2.8010P] 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^)+(0.0648P)^2^+2.8010P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322681