What is the Real Steric Impact of Triphenylphosphite? Solid-State and Solution Structural Studies ofcis- andtrans-Isomers of M(CO)4[P(OPh)3]2(M = Mo and W)
Darensbourg, Donald J.; Andreatta, Jeremy R.; Stranahan, Sarah M.; Reibenspies, Joseph H.; Organometallics 26 (2007) 6832–; doi:10.1021/om700761q

data_4073966
_publ_section_title
;
 What is the Real Steric Impact of Triphenylphosphite? Solid-State and
 Solution Structural Studies ofcis- andtrans-Isomers of M(CO)4[P(OPh)3]2(M
 = Mo and W)
;
_journal_issue                   27
_journal_name_full               Organometallics
_journal_page_first              6832
_journal_paper_doi               10.1021/om700761q
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C54 H48 N2 O14 P2 W2'
_chemical_formula_weight         1378.58
_chemical_name_systematic
; 
 ? 
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.3660(18)
_cell_length_b                   14.5829(15)
_cell_length_c                   19.565(2)
_cell_measurement_reflns_used    9537
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.06
_cell_volume                     5240.1(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.2199
_diffrn_reflns_av_sigmaI/netI    0.0903
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47056
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    4.516
_exptl_absorpt_correction_T_max  0.8057
_exptl_absorpt_correction_T_min  0.6609
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            clear/yellow
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         6.430
_refine_diff_density_min         -3.174
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          1.472
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+22.0389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1345
_reflns_number_gt                5171
_reflns_number_total             5987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700761q-file009.cif
_cod_data_source_block           ddss092606
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        5240.0(9)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4073966