Addition-Elimination Reactions across the M-C Bond of Metal N-Heterocyclic Carbenes
Zoë R. Turner; Ronan Bellabarba; Robert P. Tooze; Polly L. Arnold; Journal of the American Chemical Society 132 (2010) 4050–4051; doi:10.1021/ja910673q

data_4102181
_publ_contact_author_name        'Polly L. Arnold; Simon Parsons'
_publ_section_title
;
 Addition-Elimination Reactions across the M-C Bond of Metal
 N-Heterocyclic Carbenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4050
_journal_page_last               4051
_journal_paper_doi               10.1021/ja910673q
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C41 H80 Ce1 N7 O1 Si4'
_chemical_formula_sum            'C41 H80 Ce N7 O Si4'
_chemical_formula_weight         939.60
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-02-15
_audit_creation_method           CRYSTALS_ver_12.87
_cell_angle_alpha                90
_cell_angle_beta                 103.097(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   12.5342(7)
_cell_length_b                   65.014(3)
_cell_length_c                   21.5322(10)
_cell_measurement_reflns_used    9235
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     17090.1(15)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device       'Bruker Kappa Apex2'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       85
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            174994
_diffrn_reflns_theta_full        27.261
_diffrn_reflns_theta_max         28.397
_diffrn_reflns_theta_min         1.020
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.915
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5964
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.35
_platon_squeeze_details
;
;
_refine_diff_density_max         2.48
_refine_diff_density_min         -4.32
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1032
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1459
_refine_ls_number_reflns         27941
_refine_ls_number_restraints     330
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0951
_refine_ls_shift/su_max          0.008943
_refine_ls_structure_factor_coef F
_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: 
 75.9 36.2 56.1 39.2 14.1 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0825
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0820
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              85
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                27941
_reflns_number_total             41020
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0951
_oxford_refine_ls_scale          2.885(3)
_oxford_reflns_number_all        30078
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'po8103 in P2(1)/n'
_cod_data_source_file            ja910673q_si_008.cif
_cod_data_source_block           po8103
_cod_original_cell_volume        17090.2(15)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C41 H80 Ce1 N7 O1 Si4'
_cod_database_code               4102181