Addition of the [(tBuP)3As]− anion to the cyclopentadienyl ring of [(C5H5)M(CO)3Cl] (M = Mo, W)
Bashall, Alan; Hopkins, Alexander D.; Mays, Martin J.; McPartlin, Mary; Wood, Jody A.; Woods, Anthony D.; Wright, Dominic S.; Journal of the Chemical Society, Dalton Transactions  (2000) 1825–; doi:10.1039/b003687k

data_7009797
_publ_section_title
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 Addition of the [(tBuP)3As]&#x2212; anion to the cyclopentadienyl ring
 of [(C5H5)M(CO)3Cl] (M&#x2005;=&#x2005;Mo, W)
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_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1825
_journal_paper_doi               10.1039/b003687k
_journal_year                    2000
_chemical_formula_sum            'C20 H31 As Cl Mo O3 P3'
_chemical_formula_weight         618.67
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 91.000(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.308(2)
_cell_length_b                   16.303(4)
_cell_length_c                   10.132(2)
_cell_measurement_temperature    223(2)
_cell_volume                     2693.4(9)
_computing_cell_refinement       'BRUKERS XSCANS'
_computing_data_collection       'BRUKERS XSCANS'
_computing_data_reduction        'BRUKERS XSCANS'
_computing_molecular_graphics    'BRUKERS SHELXTL'
_computing_publication_material  'BRUKERS SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKERS P4'
_diffrn_measurement_method       theta/2theta
_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  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0677
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7944
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0.2
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.001
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8045
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         3738
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          6.391
_refine_ls_shift/su_mean         0.359
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+0.2339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0732
_reflns_number_gt                2703
_reflns_number_total             3738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b003687k.txt
_cod_data_source_block           mz410
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_original_cell_volume        2693.5(10)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7009797