N2 Hydrogenation from Activated End-On Bis(indenyl) Zirconium Dinitrogen Complexes
Doris Pun; Christopher A. Bradley; Emil Lobkovsky; Ivan Keresztes; Paul J. Chirik; Journal of the American Chemical Society 130 (2008) 14046–14047; doi:10.1021/ja8048332

data_4108547
_publ_section_title
;
 N2 Hydrogenation from Activated End-On Bis(indenyl) Zirconium Dinitrogen
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14046
_journal_page_last               14047
_journal_paper_doi               10.1021/ja8048332
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C52 H60 Cl2 N2 Na2 Zr2'
_chemical_formula_sum            'C52 H60 Cl2 N2 Na2 Zr2'
_chemical_formula_weight         1012.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2867(4)
_cell_length_b                   15.2867(4)
_cell_length_c                   23.8065(13)
_cell_measurement_reflns_used    4644
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.94
_cell_measurement_theta_min      2.17
_cell_volume                     5563.2(4)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3455
_diffrn_reflns_theta_full        22.11
_diffrn_reflns_theta_max         22.11
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  0.9035
_exptl_absorpt_correction_T_min  0.8601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3455
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+0.1914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0995
_reflns_number_gt                3004
_reflns_number_total             3455
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8048332_si_003.cif
_cod_data_source_block           cb53
_cod_depositor_comments
;

2021-08-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C104 H120 Cl4 N4 Na4 Zr4'
_cod_original_formula_weight         2024.68
_cod_original_formula_moiety         'C104 H120 Cl4 N4 Na4 Zr4'
_cod_original_formula_units_Z            2
_cod_database_code               4108547