Snapshots of an Alkylidyne for Nitride Triple-Bond Metathesis
Brad C. Bailey; Alison R. Fout; Hongjun Fan; John Tomaszewski; John C. Huffman; J. Brannon Gary; Marc J. A. Johnson; Daniel J. Mindiola; Journal of the American Chemical Society 129 (2007) 2234–2235; doi:10.1021/ja0689684

data_4109128
_publ_section_title
;
 Snapshots of an Alkylidyne for Nitride Triple-Bond Metathesis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2234
_journal_page_last               2235
_journal_paper_doi               10.1021/ja0689684
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C31.5 H55 Cl N2 P2 Si Ti'
_chemical_formula_weight         635.16
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.14(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.655(2)
_cell_length_b                   41.822(8)
_cell_length_c                   14.864(3)
_cell_measurement_reflns_used    1973
_cell_measurement_temperature    126(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.28
_cell_volume                     7226(2)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_molecular_graphics    'Reciprocal Net (http://recipnet.org)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      126(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
'   0.30 degree frames measured for  10.16 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w 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  0.0853
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            126661
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.454
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       'cleaved fragment'
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.889
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1123
_refine_ls_number_reflns         16634
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                10983
_reflns_number_total             16634
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0689684si20061214_062350.cif
_cod_data_source_block           06162
_cod_original_cell_volume        7226(3)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C31.50 H55 Cl N2 P2 Si Ti'
_cod_database_code               4109128