Reversible 1,2-Alkyl Migration to Carbene and Ammonia Activation in an NHC-Zirconium Complex.
Despagnet-Ayoub, Emmanuelle; Takase, Michael K.; Labinger, Jay A.; Bercaw, John E.; Journal of the American Chemical Society  (2015) 150817104804004–; doi:10.1021/jacs.5b06695

data_4124280
_publ_section_title
;
 Reversible 1,2-Alkyl Migration to Carbene and Ammonia Activation in an
 NHC-Zirconium Complex.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              150817104804004
_journal_paper_doi               10.1021/jacs.5b06695
_journal_year                    2015
_chemical_formula_sum            'C97.97 H145.53 N8 O4 Zr2'
_chemical_formula_weight         1681.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.3251(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.6453(7)
_cell_length_b                   19.6437(5)
_cell_length_c                   19.8192(6)
_cell_measurement_reflns_used    9234
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.62
_cell_measurement_theta_min      2.88
_cell_volume                     9594.8(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 v2014.7-1 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker-AXS, 2007)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (She ldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1244
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            177942
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.913
_diffrn_reflns_theta_min         2.877
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.172
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/4 (Sheldrick, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3605
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.282
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1232
_refine_ls_number_reflns         19668
_refine_ls_number_restraints     897
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+27.0617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14985
_reflns_number_total             19668
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b06695_si_002.cif
_cod_data_source_block           P15063
_cod_database_code               4124280
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.671
_shelx_estimated_absorpt_t_max   0.899
_shelx_res_checksum              9660
_shelx_hkl_checksum              91075