Synthesis and Characterization of (2,6-iPrNCN)HfCl2-and (3,5-MeNCN)2Hf2-(where NCN = 2,6-bis[phenylazanidyl]methylphenyl): New Trianionic Pincer Ligands
Koller, Jürgen; Sarkar, Soumya; Abboud, Khalil A.; Veige, Adam S.; Organometallics 26 (2007) 5438–; doi:10.1021/om700597u

data_4073745
_publ_section_title
;
 Synthesis and Characterization of (2,6-iPrNCN)HfCl2-and
 (3,5-MeNCN)2Hf2-(where NCN =
 2,6-bis[phenylazanidyl]methylphenyl):&#x00A0; New Trianionic Pincer
 Ligands
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5438
_journal_paper_doi               10.1021/om700597u
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C44 H71 Cl2 Hf Li N2 O6'
_chemical_formula_weight         980.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 98.627(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2626(11)
_cell_length_b                   12.6991(10)
_cell_length_c                   27.443(2)
_cell_measurement_reflns_used    67
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     4914.3(6)
_computing_cell_refinement
'Bruker SMART v5.624 & SAINT 6.36a (Bruker 1998)'
_computing_data_collection       'Bruker SMART v5.624 (Bruker 1998)'
_computing_data_reduction        'Bruker SHELXTL v6.14 (Bruker 2000)'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement  'Bruker SHELXTL v6.14'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'SMART CCD area detector'
_diffrn_measurement_method       '\w 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  0.1139
_diffrn_reflns_av_sigmaI/netI    0.1526
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            31825
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.274
_exptl_absorpt_correction_T_max  0.8889
_exptl_absorpt_correction_T_min  0.8220
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.12 (Bruker 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.398
_refine_diff_density_min         -1.283
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         11123
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1439
_refine_ls_R_factor_gt           0.0704
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1669
_reflns_number_gt                6300
_reflns_number_total             11123
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om700597u-file002.cif
_cod_data_source_block           kv26
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        4914.3(7)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4073745