Nitratotris(2,2,6,6-tetramethyl-3,5-heptadionato)hafnium(IV)
Urs, Usha K.; Dharmaprakash, M. S.; Shivashankar, S. A.; Guru Row, T. N.; Acta Crystallographica Section E 59 (2003) m1–m2; doi:10.1107/S160053680202202X

data_2201842
_publ_section_title
;
 Nitratotris(2,2,6,6-tetramethyl-3,5-heptadionato)hafnium(IV)
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1
_journal_page_last               m2
_journal_paper_doi               10.1107/S160053680202202X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Hf (C11 H19 O2)3 (N O3)]'
_chemical_formula_moiety         'C33 H57 Hf N O9'
_chemical_formula_sum            'C33 H57 Hf N O9'
_chemical_formula_weight         790.29
_chemical_name_systematic
;
Nitratotris(2,2,6,6-tetramethyl-3,5-heptadionato)hafnium(IV)
;
_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           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                79.683(16)
_cell_angle_beta                 75.336(16)
_cell_angle_gamma                83.579(16)
_cell_formula_units_Z            2
_cell_length_a                   10.156(9)
_cell_length_b                   10.590(9)
_cell_length_c                   19.277(17)
_cell_measurement_reflns_used    21660
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.63
_cell_measurement_theta_min      1.11
_cell_volume                     1968(3)
_computing_cell_refinement       'SAINT (Bruker, 1998'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       \w
_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  0.092
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21660
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         1.11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.695
_exptl_absorpt_correction_T_max  0.538
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.506
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         8429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0539P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                4904
_reflns_number_total             8429
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf6224.cif
_cod_data_source_block           I
_cod_original_cell_volume        1969(3)
_cod_database_code               2201842
_cod_database_fobs_code          2201842