Crystal structures of <i>trans</i>-acetyldicarbonyl(<i>{η</i>}^5^-cyclopentadienyl)(dimethylphenylphosphane)molybdenum(II) and <i>trans</i>-acetyldicarbonyl(<i>{η</i>}^5^-cyclopentadienyl)(ethyldiphenylphosphane)molybdenum(II)
Whited, Matthew T.; Hofmeister, Gretchen E.; Hodges, Connor J.; Jensen, Laramie T.; Keyes, Samuel H.; Ngamnithiporn, Aurapat; Janzen, Daron E.; Acta Crystallographica Section E 70 (2014) 216–220; doi:10.1107/S1600536814020534

data_2240025
_publ_section_title
;
 Crystal structures of
 <i>trans</i>-acetyldicarbonyl(<i>{\h</i>}^5^-cyclopentadienyl)(dimethylphenylphosphane)molybdenum(II)
 and
 <i>trans</i>-acetyldicarbonyl(<i>{\h</i>}^5^-cyclopentadienyl)(ethyldiphenylphosphane)molybdenum(II)
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              216
_journal_page_last               220
_journal_paper_doi               10.1107/S1600536814020534
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Mo (C8 H11 P) (C5 H5) (C2 H3 O) (C O)2]'
_chemical_formula_moiety         'C17 H19 Mo O3 P'
_chemical_formula_sum            'C17 H19 Mo O3 P'
_chemical_formula_weight         398.23
_chemical_name_systematic
;
<i>trans</i>-Acetyldicarbonyl-(<i>\h</i>^5^-cyclopentadienyl)-\\
(dimethylphenylphosphine)-molybdenum(II)
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.23 svn.r2946 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.374(2)
_cell_length_b                   6.8898(10)
_cell_length_c                   15.208(2)
_cell_measurement_reflns_used    16109
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      3.21
_cell_volume                     1715.7(4)
_computing_cell_refinement       'CrystalClear (Rigaku, 2011)'
_computing_data_collection       'CrystalClear (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear (Rigaku, 2011)'
_computing_molecular_graphics    'Olex2 (Dolomanov <i>et al.</i>, 2009)'
_computing_publication_material  'Olex2 (Dolomanov <i>et al.</i>, 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 6.849
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17021
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.208
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>REQAB</i>; Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.265
_refine_ls_abs_structure_details
;
Flack x determined using 1649 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013).
;
_refine_ls_abs_structure_Flack   0.007(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3923
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0142P)^2^+0.4930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0435
_refine_ls_wR_factor_ref         0.0447
_reflns_number_gt                3639
_reflns_number_total             3923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5058sup1.cif
_cod_data_source_block           1
_cod_original_cell_volume        1715.6(4)
_cod_database_code               2240025
_cod_database_fobs_code          2240025
_shelx_hkl_checksum              90740
_shelx_res_checksum              52679