Trichlorido{methyl[4-(methylimino)pent-2-en-2-yl]azanido-κ^2^<i>N</i>,<i>N</i>'}hafnium(IV)
Ikeda, Ken; Masuda, Hideki; Acta Crystallographica Section E 69 (2013) m505–; doi:10.1107/S1600536813022745

data_2238465
_publ_section_title
;
 Trichlorido{methyl[4-(methylimino)pent-2-en-2-yl]azanido-\k^2^<i>N</i>,<i>N</i>'}hafnium(IV)
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m505
_journal_paper_doi               10.1107/S1600536813022745
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Hf (C29 H41 N2) Cl3]'
_chemical_formula_moiety         'C29 H41 Cl3 Hf N2'
_chemical_formula_sum            'C29 H41 Cl3 Hf N2'
_chemical_formula_weight         702.51
_chemical_name_systematic
Trichlorido{methyl[4-(methylimino)pent-2-en-2-yl]azanido-\k^2^<i>N</i>,<i>N</i>'}hafnium(IV)
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.980(3)
_cell_length_b                   21.808(4)
_cell_length_c                   9.8492(16)
_cell_measurement_reflns_used    7615
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.15
_cell_volume                     3002.8(10)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2006)'
_computing_molecular_graphics    'CrystalStructure (Rigaku/MSC, 2006)'
_computing_publication_material  'CrystalStructure (Rigaku/MSC, 2006)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            22083
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.754
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             1408.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.650
_refine_diff_density_min         -1.020
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    0
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3527
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0262P)^2^+3.9270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0684
_reflns_number_gt                3132
_reflns_number_total             3527
_reflns_threshold_expression     F^2^>2\s(F^2^)
_cod_data_source_file            bh2479.cif
_cod_data_source_block           I
_cod_original_cell_volume        3002.8(9)
_cod_database_code               2238465
_cod_database_fobs_code          2238465