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_4332588
_publ_contact_author
;
                             ? # Name and address of author for correspondence
;
_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
;
?
;
_chemical_formula_moiety         ' C36 H31 O2 P2 W2 1+,  B1 F4 1- , H2 O'
_chemical_formula_sum            'C36 H33 B F4 O3 P2 W2'
_chemical_formula_weight         1030.1
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             01-01-25
_audit_creation_method           CRYSTALS
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   40.032(10)
_cell_length_b                   40.032(10)
_cell_length_c                   9.257(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      14.2
_cell_measurement_theta_min      14
_cell_volume                     14835(11)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;
RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)
;
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_diffrn_ambient_temperature      295
_diffrn_measurement_device       'Enraf-nonius CAD4'
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7161
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        5.8
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    6.47
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '\y scan'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.84
_exptl_crystal_description       stick
_exptl_crystal_F_000             7781.69
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.11
_refine_diff_density_min         -0.95
_refine_ls_extinction_coef       26
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   1.0343
_refine_ls_hydrogen_treatment
;
 H atoms placed geometrically after each cycle
 one overall isotropic thermal parameter refined
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         3560
_refine_ls_R_factor_obs          0.0485
_refine_ls_shift/esd_max         0.526081
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;
 Chebychev polynomial (Carruthers & Watkin, 1979)
 Three coefficients 10.9, -6.36, and 7.68
;
_refine_ls_wR_factor_obs         0.0556
_reflns_number_observed          3560
_reflns_number_total             6500
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ic060544nsup1.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_cell_measurement_temperature' value '295K' was changed to '295' -
the value should be numeric and without a unit
designator.

'_diffrn_ambient_temperature' value '295K' was changed
to '295' - the value should be numeric and without a unit
designator.

'_symmetry_cell_setting' value 'Tetragonal ' changed to
'tetragonal' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'EMPIRICAL'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct_Methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'Geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      'I 41/a '
_cod_original_formula_sum        ' C36 H33 B1 F4 O3 P2 W2   '
_cod_database_code               4332588