Direct Reaction of Aroyl Cyanides with Azazirconacyclopentadienes: Synthesis and Structural Characterization of Stabilized Azazirconacyclopentenes
Liu, Yuanhong; Yan, Bin; Organometallics 25 (2006) 544–; doi:10.1021/om0506264

data_4074619
_publ_section_title
;
 Direct Reaction of Aroyl Cyanides with
 Azazirconacyclopentadienes:&#x00A0; Synthesis and Structural
 Characterization of Stabilized Azazirconacyclopentenes
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              544
_journal_paper_doi               10.1021/om0506264
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C30 H36 N2 O Zr'
_chemical_formula_weight         531.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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            8
_cell_length_a                   16.8549(16)
_cell_length_b                   37.450(4)
_cell_length_c                   8.5661(8)
_cell_measurement_reflns_used    2728
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      41.016
_cell_measurement_theta_min      5.299
_cell_volume                     5407.1(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_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  0.1171
_diffrn_reflns_av_sigmaI/netI    0.0997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            30162
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83909
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.351
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.00113(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.091
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1450
_reflns_number_gt                2916
_reflns_number_total             5893
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0506264si20050725_105223.cif
_cod_data_source_block           cd2593
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Pccn
_cod_database_code               4074619