High Yield Synthesis and Reactivity of a Phosphinidene Bridged Dimolybdenum Complex
M. Esther García; Víctor Riera; Miguel A. Ruiz; David Sáez; Jacqueline Vaissermann; John C. Jeffery; Journal of the American Chemical Society 124 (2002) 14304–14305; doi:10.1021/ja021072o

data_4115343
_publ_contact_author             'Ruiz, Miguel A.'
_publ_contact_author_email       ' mara@sauron.quimica.uniovi.es '
_publ_contact_author_fax         ' 34 985 103446 '
_publ_section_title
;
 High Yield Synthesis and Reactivity of a Phosphinidene Bridged
 Dimolybdenum Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14304
_journal_page_last               14305
_journal_paper_doi               10.1021/ja021072o
_journal_volume                  124
_journal_year                    2002
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C32 H39 Mo2 O4 P1 '
_chemical_formula_sum            'C32 H39 Mo2 O4 P'
_chemical_formula_weight         710.50
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 98.05(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.630(2)
_cell_length_b                   13.612(3)
_cell_length_c                   16.663(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      12.3
_cell_measurement_theta_min      12
_cell_volume                     3061.0(14)
_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  0.03
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6554
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        16.23
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.88
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '\y scan'
_exptl_crystal_colour            ' red '
_exptl_crystal_density_diffrn    1.54
_exptl_crystal_description       prism
_exptl_crystal_F_000             1429.67
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.94
_refine_diff_density_min         -1.35
_refine_ls_extinction_coef       354
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   0.9867
_refine_ls_hydrogen_treatment
;
 H atoms placed geometrically after each cycle
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         3309
_refine_ls_R_factor_obs          0.0599
_refine_ls_shift/esd_max         0.089113
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;
 Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_wR_factor_obs         0.0749
_reflns_number_observed          3309
_reflns_number_total             6008
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ja021072o_s1_1.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
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_cell_volume        3061(1)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C32 H39 Mo2 O4 P1 '
_cod_database_code               4115343