Oxygen Atom Transfer Reactivity from a Dioxo-Mo(VI) Complex to Tertiary Phosphines: Synthesis, Characterization, and Structure of Phosphoryl Intermediate Complexes
Victor N. Nemykin; Partha Basu; Inorganic Chemistry 44 (2005) 7494–7502; doi:10.1021/ic0508324

data_4309758
_publ_contact_author_address
; 
 Department of Chemistry, 
 University of Minnesota Duluth, 
 1039 University Drive, 
 Duluth, MN, 55812, USA. 
;
_publ_contact_author_email       vnemykin@d.umn.edu
_publ_contact_author_fax         '+1 218 7267394'
_publ_contact_author_name        'Victor Nemykin'
_publ_contact_author_phone       '+1 218 7266729'
_publ_section_title
;
Oxygen Atom Transfer Reactivity from a Dioxo-Mo(VI) Complex to Tertiary
Phosphines: Synthesis, Characterization, and Structure of Phosphoryl
Intermediate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7494
_journal_page_last               7502
_journal_paper_doi               10.1021/ic0508324
_journal_volume                  44
_journal_year                    2005
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C29 H39 B1 Cl1 Mo1 N6 O2 P1'
_chemical_formula_sum            'C29 H39 B Cl Mo N6 O2 P'
_chemical_formula_weight         676.85
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-03-04
_audit_creation_method           CRYSTALS_ver_12.39
_cell_angle_alpha                90
_cell_angle_beta                 91.88(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.67(3)
_cell_length_b                   16.59(2)
_cell_length_c                   14.722(15)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      14
_cell_measurement_theta_min      10
_cell_volume                     3337(9)
_computing_cell_refinement       'Rigaku AFC-7R'
_computing_data_collection       'Rigaku AFC-7R'
_computing_data_reduction        'TeXsan 10.1b'
_computing_molecular_graphics    'CAMERON (Watkin et al 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al 1996)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC-7R'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3953
_diffrn_reflns_theta_full        27.505
_diffrn_reflns_theta_max         27.505
_diffrn_reflns_theta_min         2.769
_diffrn_standards_decay_%        3.00
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
; 
 Azimutal absorption correction (North et al, 1968) 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       prism
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.78
_refine_diff_density_min         -0.66
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9845
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         1673
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.2369
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.003200
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 11.4 11.1 7.41 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2341
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.1599
_reflns_limit_h_max              17
_reflns_limit_h_min              0
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              -19
_reflns_number_gt                1673
_reflns_number_total             3821
_reflns_threshold_expression     I>2.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.10512(9)
_oxford_structure_analysis_title 'TeXsan on Shelx'
_cod_data_source_file            ic0508324si20050523_113135_2.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C 1 c 1 '
_cod_original_formula_sum        'C29 H39 B1 Cl1 Mo1 N6 O2 P1'
_cod_database_code               4309758