Factors Influencing Coordination versus Oxidative Addition of C−H Bonds to Molybdenum and Tungsten: Structural and Spectroscopic Evidence That the Calixarene Framework Promotes C−H Bond Activation
Buccella, Daniela; Tanski, Joseph M.; Parkin, Gerard; Organometallics 26 (2007) 3275–; doi:10.1021/om700279c

data_4073338
_publ_section_title
;
 Factors Influencing Coordination versus Oxidative Addition of C&#x2212;H
 Bonds to Molybdenum and Tungsten:&#x00A0; Structural and Spectroscopic
 Evidence That the Calixarene Framework Promotes C&#x2212;H Bond
 Activation
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_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3275
_journal_paper_doi               10.1021/om700279c
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C26 H47 O2 P3 W'
_chemical_formula_weight         668.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.5290(10)
_cell_angle_beta                 76.5570(10)
_cell_angle_gamma                80.4750(10)
_cell_formula_units_Z            2
_cell_length_a                   8.73650(10)
_cell_length_b                   11.2335(2)
_cell_length_c                   15.7357(2)
_cell_measurement_reflns_used    9324
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      38.77
_cell_measurement_theta_min      2.51
_cell_volume                     1468.45(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      115(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0171
_diffrn_reflns_av_sigmaI/netI    0.0154
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22287
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    4.116
_exptl_absorpt_correction_T_max  0.5772
_exptl_absorpt_correction_T_min  0.3525
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Bulk
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.757
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_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         5980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0144
_refine_ls_R_factor_gt           0.0139
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+1.3378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0358
_refine_ls_wR_factor_ref         0.0360
_reflns_number_gt                5828
_reflns_number_total             5980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700279c-file002.cif
_cod_data_source_block           lwp3h3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4073338