Migratory Insertion Reactions in Asymmetrical Guanidinate-Supported Zirconium Complexes
Fernández-Galán, Rafael; Antiñolo, Antonio; Carrillo-Hermosilla, Fernando; López-Solera, Isabel; Otero, Antonio; Serrano-Laguna, Amparo; Villaseñor, Elena; Organometallics 31 (2012) 8360–; doi:10.1021/om300942p

data_4079687
_publ_section_title
;
 Migratory Insertion Reactions in Asymmetrical Guanidinate-Supported
 Zirconium Complexes
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              8360
_journal_paper_doi               10.1021/om300942p
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C64 H88 N8 Zr'
_chemical_formula_weight         1060.64
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.863(3)
_cell_angle_beta                 79.891(3)
_cell_angle_gamma                75.840(3)
_cell_formula_units_Z            2
_cell_length_a                   11.8113(7)
_cell_length_b                   16.1538(8)
_cell_length_c                   16.9957(11)
_cell_measurement_reflns_used    4193
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      23.1402
_cell_measurement_theta_min      2.5239
_cell_volume                     2985.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_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      260(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega and phi 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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0920
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31506
_diffrn_reflns_theta_full        30.70
_diffrn_reflns_theta_max         30.70
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.530
_exptl_crystal_size_mid          0.473
_exptl_crystal_size_min          0.452
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0001(6)
_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   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         18065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1663
_reflns_number_gt                10808
_reflns_number_total             18065
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300942p_si_003.cif
_cod_data_source_block           9
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4079687