Preparation and Characterization of Bis[(μ-acetato)halo(μ-bis(diphenylphosphino)amine)molybdenum(II)] Complexes
Deirdre I. Arnold; F. Albert Cotton; Fritz E. Kühn; Inorganic Chemistry 35 (1996) 4733–4737; doi:10.1021/ic9514758

data_4323867
_publ_section_title
;
 Preparation and Characterization of
 Bis[(\m-acetato)halo(\m-bis(diphenylphosphino)amine)molybdenum(II)]
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4733
_journal_page_last               4737
_journal_paper_doi               10.1021/ic9514758
_journal_volume                  35
_journal_year                    1996
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C56 H60 Cl2 Mo2 N2 O6 P4'
_chemical_formula_structural
'(Mo Cl (C2 H3 O2)(C24 H21 N P2))2 2(C2 H6 O)'
_chemical_formula_sum            'C56 H60 Cl2 Mo2 N2 O6 P4'
_chemical_formula_weight         1243.76
_chemical_name_systematic
;
 Di[(\m-acetato)chloro(\m-bis(diphenylphosphino)amine)molybdenum(III)]
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c 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                   16.830(2)
_cell_length_b                   20.310(4)
_cell_length_c                   16.751(2)
_cell_measurement_reflns_used    75
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      25
_cell_volume                     5725.8(15)
_computing_cell_refinement       'LCR (Ulm, 1992)'
_computing_data_collection       AFC5R
_computing_data_reduction        'MSC Texsan'
_computing_molecular_graphics    'ORTEP (Ulm, 1992)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       AFC5R-Rigaku
_diffrn_measurement_method       Omega/2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0786
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3265
_diffrn_reflns_theta_max         52.50
_diffrn_reflns_theta_min         4.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'based on interval count'
_diffrn_standards_interval_time  30.2
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.899
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'tiny blocks'
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.189
_refine_diff_density_min         -1.326
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.052
_refine_ls_goodness_of_fit_obs   1.139
_refine_ls_hydrogen_treatment    'HFIX 137 riding on pivotal C, common U'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         2807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_restrained_S_obs      1.139
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_obs          0.0561
_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^)+(0.0987P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1641
_refine_ls_wR_factor_obs         0.1400
_reflns_number_observed          2217
_reflns_number_total             3265
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9514758_2.cif
_cod_data_source_block           Mo2Cl2(dppa)2(Ac)2_2(C2H5OH)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0987P)^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^)+(0.0987P)^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 
;
_cod_original_cell_volume        5725.8(16)
_cod_database_code               4323867