Diazene Dehydrogenation Follows H2 Addition to Coordinated Dinitrogen in anansa-Zirconocene Complex
Tamara E. Hanna; Ivan Keresztes; Emil Lobkovsky; Paul J. Chirik; Inorganic Chemistry 46 (2007) 1675–1683; doi:10.1021/ic0620539

data_4307553
_publ_section_title
;
Diazene Dehydrogenation Follows H2 Addition to Coordinated Dinitrogen in
anansa-Zirconocene Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1675
_journal_page_last               1683
_journal_paper_doi               10.1021/ic0620539
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C40 H62 N2 Si2 Zr2'
_chemical_formula_sum            'C40 H62 N2 Si2 Zr2'
_chemical_formula_weight         809.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.714(5)
_cell_angle_beta                 92.826(5)
_cell_angle_gamma                106.954(4)
_cell_formula_units_Z            2
_cell_length_a                   11.0951(13)
_cell_length_b                   12.6629(17)
_cell_length_c                   15.319(2)
_cell_measurement_reflns_used    6695
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     2045.7(5)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38481
_diffrn_reflns_theta_full        31.80
_diffrn_reflns_theta_max         31.80
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  0.9708
_exptl_absorpt_correction_T_min  0.9159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         13747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0676
_reflns_number_gt                10812
_reflns_number_total             13747
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0620539si20061026_021501.cif
_cod_data_source_block           th12
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2045.6(5)
_cod_database_code               4307553