Imino phenoxide complexes of group 4 metals: synthesis, structural characterization and polymerization studies
Saha, Tanmoy Kumar; Mandal, Mrinmay; Chakraborty, Debashis; Ramkumar, Venkatachalam; New Journal of Chemistry 37 (2013) 949–; doi:10.1039/c3nj40916c

data_7053034
_publ_section_title
;
 Imino phenoxide complexes of group 4 metals: synthesis, structural
 characterization and polymerization studies
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              949
_journal_paper_doi               10.1039/c3nj40916c
_journal_volume                  37
_journal_year                    2013
_chemical_formula_moiety         'C41 H68 Hf N2 O4'
_chemical_formula_sum            'C41 H68 Hf N2 O4'
_chemical_formula_weight         831.46
_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                88.239(2)
_cell_angle_beta                 85.703(2)
_cell_angle_gamma                79.019(2)
_cell_formula_units_Z            8
_cell_length_a                   16.4326(9)
_cell_length_b                   21.7830(11)
_cell_length_c                   25.0841(13)
_cell_measurement_temperature    298(2)
_cell_volume                     8788.5(8)
_computing_cell_refinement       'APEXII/SAINT (Bruker, 2004)'
_computing_data_collection       'APEXII (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997) '
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            118536
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.55
_diffrn_reflns_theta_min         0.81
_exptl_absorpt_coefficient_mu    2.411
_exptl_absorpt_correction_T_max  0.0971
_exptl_absorpt_correction_T_min  0.0516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker,2004)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             9638
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         13.489
_refine_diff_density_min         -2.159
_refine_diff_density_rms         0.243
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.219
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1810
_refine_ls_number_reflns         42436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.219
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.2200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1507
_refine_ls_wR_factor_ref         0.1779
_reflns_number_gt                29967
_reflns_number_total             42436
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj40916c.txt
_cod_data_source_block           Hf
_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.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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               7053034