Investigation of Zr-C, Zr-N, and Potential Agostic Interactions in an Organozirconium Complex by Experimental Electron Density Analysis
Sebastien Pillet; Guang Wu; Vichien Kulsomphob; Benjamin G. Harvey; Richard D. Ernst; Philip Coppens; Journal of the American Chemical Society 125 (2003) 1937–1949; doi:10.1021/ja021133i

data_4113459
_publ_contact_author_address
;
Department of Chemistry, University of New York at Buffalo, 
Buffalo, New York 14260
;
_publ_contact_author_email       ' coppens@acsu.buffalo.edu'
_publ_contact_author_name        ' Philip Coppens'
_publ_section_title
;
 Investigation of Zr-C, Zr-N, and Potential Agostic Interactions in an
 Organozirconium Complex by Experimental Electron Density Analysis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1937
_journal_page_last               1949
_journal_paper_doi               10.1021/ja021133i
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C24 H35 N Zr'
_chemical_formula_sum            'C24 H35 N Zr'
_chemical_formula_weight         428.7672
_chemical_name_common
;
 ?                                                         
;
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.482(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5981(4)
_cell_length_b                   9.3991(5)
_cell_length_c                   27.0670(9)
_cell_measurement_reflns_used    41631
_cell_measurement_temperature    16
_cell_measurement_theta_max      48.09
_cell_measurement_theta_min      1.35
_cell_volume                     2168.78(17)
_computing_cell_refinement       SAINT
_computing_data_collection       SAINT
_computing_data_reduction        'SORTAV (Blessing, 1989)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      16
_diffrn_measured_fraction_theta_full 0.48
_diffrn_measured_fraction_theta_max 0.48
_diffrn_measurement_device_type  'Smart CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6361
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_sigmaI/netI    0.2280
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            41631
_diffrn_reflns_theta_full        48.09
_diffrn_reflns_theta_max         48.26
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    2.16
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Absorption correction were performed using SORTAV (Blessing 1989) 
;
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       irregular
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.76
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1211
_refine_ls_number_reflns         13948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.76
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 'calc w=1/[\s^2^(Fo)]' 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0158
_refine_ls_wR_factor_ref         0.0158
_reflns_number_gt                10912
_reflns_number_total             13948
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            ja021133i.cif
_cod_data_source_block           Zr-compound
_cod_original_cell_volume        2168.8(2)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4113459