Chemistry of the Oxophosphinidene Ligand. 1. Electronic Structure of the Anionic Complexes [MCp{P(O)R*}(CO)2]- (M = Mo, W; R* = 2,4,6-C6H2tBu3) and Their Reactions with H+ and C-Based Electrophiles.
María Alonso; M. Angeles Alvarez; M. Esther García; Daniel García-Vivó; Miguel A. Ruiz; Inorganic Chemistry 49 (2010) 8962–8976; doi:10.1021/ic101261f

data_4316621
_publ_section_title
;
 Chemistry of the Oxophosphinidene Ligand. 1. Electronic Structure of the
 Anionic Complexes [MCp{P(O)R*}(CO)2]- (M = Mo, W; R* = 2,4,6-C6H2tBu3)
 and Their Reactions with H+ and C-Based Electrophiles.
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8962
_journal_page_last               8976
_journal_paper_doi               10.1021/ic101261f
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C34 H51 Mo N2 O3 P'
_chemical_formula_weight         662.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   9.5709(15)
_cell_length_b                   17.391(3)
_cell_length_c                   20.501(3)
_cell_measurement_temperature    173.5
_cell_volume                     3412.3(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.5
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0891
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22309
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.465
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         7820
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.243
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                5105
_reflns_number_total             7820
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101261f_si_002_1.cif
_cod_data_source_block           comp3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/adriana/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_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_cell_measurement_temperature' value '173.5K' was changed to '173.5'
- the value should be numeric and without a unit
designator.

'_diffrn_ambient_temperature' value '173.5K' was changed
to '173.5' - the value should be numeric and without a unit
designator.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        3412.4(9)
_cod_database_code               4316621