Synthesis and Structural Diversity of Group 4 Metal Complexes with Multidentate Tethered Phenoxy-Amidine and Phenoxy-Amidinate Ligands
Kirillov, Evgeny; Roisnel, Thierry; Carpentier, Jean-François; Organometallics 31 (2012) 3228–; doi:10.1021/om300076j

data_4078076
_publ_section_title
;
 Synthesis and Structural Diversity of Group 4 Metal Complexes with
 Multidentate Tethered Phenoxy-Amidine and Phenoxy-Amidinate Ligands
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              3228
_journal_paper_doi               10.1021/om300076j
_journal_volume                  31
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C60 H76 N2 O Zr, C6 H6'
_chemical_formula_sum            'C66 H82 N2 O Zr'
_chemical_formula_weight         1010.56
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2009-09-09T10:21:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                72.5600(10)
_cell_angle_beta                 86.7670(10)
_cell_angle_gamma                76.7770(10)
_cell_formula_units_Z            2
_cell_length_a                   12.9630(3)
_cell_length_b                   13.2343(4)
_cell_length_c                   17.9935(5)
_cell_measurement_reflns_used    78814
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     2866.67(14)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.791054E-1
_diffrn_orient_matrix_UB_12      0.202329E-1
_diffrn_orient_matrix_UB_13      -0.46066E-2
_diffrn_orient_matrix_UB_21      0.52727E-2
_diffrn_orient_matrix_UB_22      0.240686E-1
_diffrn_orient_matrix_UB_23      -0.580907E-1
_diffrn_orient_matrix_UB_31      -0.5187E-3
_diffrn_orient_matrix_UB_32      -0.749432E-1
_diffrn_orient_matrix_UB_33      -0.12196E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50672
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         13102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+1.3836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.086
_reflns_number_gt                11001
_reflns_number_total             13102
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300076j_si_001.cif
_cod_data_source_block           2
_cod_database_code               4078076