M−P versus MM Bonds as Protonation Sites in the Organophosphide-Bridged Complexes [M2Cp2(μ-PR2)(μ-PR‘2)(CO)2], (M = Mo, W; R, R‘ = Ph, Et, Cy)†
Alvarez, M. Angeles; García, M. Esther; Martínez, M. Eugenia; Ramos, Alberto; Ruiz, Miguel A.; Sáez, David; Vaissermann, Jacqueline; Inorganic Chemistry 45 (2006) 6965–6978; doi:10.1021/ic060544n

data_4332591
_publ_section_title
;
 M&#x2212;P versus MM Bonds as Protonation Sites in the
 Organophosphide-Bridged Complexes [M2Cp2(\m-PR2)(\m-PR&#x2018;2)(CO)2],
 (M = Mo, W; R, R&#x2018; = Ph, Et, Cy)&#x2020;
;
_journal_issue                   17
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6965
_journal_page_last               6978
_journal_paper_doi               10.1021/ic060544n
_journal_volume                  45
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H57 B1 Cl2 F4 Mo2 O1 P2'
_chemical_formula_sum            'C36 H57 B Cl2 F4 Mo2 O P2'
_chemical_formula_weight         917.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2005-07-22T18:28:54-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.866(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.539(7)
_cell_length_b                   17.452(10)
_cell_length_c                   19.755(12)
_cell_measurement_reflns_used    917
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      21.47
_cell_measurement_theta_min      2.3
_cell_measurement_wavelength     0.71073
_cell_volume                     3973(4)
_computing_cell_refinement       'Brucker Smart'
_computing_data_collection       'Brucker Smart'
_computing_data_reduction        'Brucker Smart'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (1999)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.92
_diffrn_measured_fraction_theta_max 0.92
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1834
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            26302
_diffrn_reflns_theta_full        24.91
_diffrn_reflns_theta_max         24.91
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.7055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER Sadabs'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.293
_refine_diff_density_min         -1.25
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.97
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6044
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1477
_refine_ls_R_factor_gt           0.0856
_refine_ls_shift/su_max          0.921
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1151P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1932
_refine_ls_wR_factor_ref         0.2181
_reflns_number_gt                4557
_reflns_number_total             6044
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060544nsup4.cif
_cod_data_source_block           mr13ee5n
_cod_depositor_comments
;
The following automatic conversions were performed:
'_diffrn_radiation_monochromador' tag replaced with
'_diffrn_radiation_monochromator'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_database_code               4332591