Reaction of Ketones with 1,4-Diaza-1,3-diene Zirconium and Hafnium Complexes: First Example of a 1,3-Dipolar Cycloaddition Reaction of 1,4-Diaza-1,3-diene Complexes of Early Transition Metals
Joachim Scholz; Helmar Görls; Inorganic Chemistry 35 (1996) 4378–4382; doi:10.1021/ic950513k

data_4323854
_publ_contact_author
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        Joachim Scholz
        Institut f\"r Anorganische Chemie
        Martin Luther Universit\"at Halle
        Geusaer Str. 
        D-06217 Merseburg
        Germany
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_publ_contact_author_fax         '03461 46-2033 '
_publ_contact_author_phone       '03461 46-2028 '
_publ_section_title
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 Reaction of Ketones with 1,4-Diaza-1,3-diene Zirconium and Hafnium
 Complexes: First Example of a 1,3-Dipolar Cycloaddition Reaction of
 1,4-Diaza-1,3-diene Complexes of Early Transition Metals
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4378
_journal_page_last               4382
_journal_paper_doi               10.1021/ic950513k
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C36 H56 N4 O2 Zr'
_chemical_formula_weight         668.07
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                93.80(3)
_cell_angle_beta                 99.84(3)
_cell_angle_gamma                106.12(3)
_cell_formula_units_Z            2
_cell_length_a                   10.395(2)
_cell_length_b                   10.865(2)
_cell_length_c                   16.842(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      23.5
_cell_measurement_theta_min      19.2
_cell_volume                     1787.4(7)
_computing_cell_refinement       SET4
_computing_data_collection       CAD4-EXPRESS
_computing_data_reduction        MOLEN
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       omega-2theta
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8771
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        -1.2
_diffrn_standards_interval_time  600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.343
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       quader
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.937
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.075
_refine_ls_goodness_of_fit_obs   1.057
_refine_ls_hydrogen_treatment    isotropical
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         7584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_restrained_S_obs      1.057
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_obs          0.0359
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+1.1858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1082
_refine_ls_wR_factor_obs         0.1015
_reflns_number_observed          6963
_reflns_number_total             7585
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic950513k_2.cif
_cod_data_source_block           FO225
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+1.1858P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+1.1858P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1787.4(6)
_cod_database_code               4323854