Dichlorido-1κ<i>Cl</i>,3κ<i>Cl</i>-hexakis[1,1,2,2,3,3(η^5^)-methylcyclopentadienyl]di-μ~2~-oxido-1:2κ^2^<i>O</i>:<i>O</i>;2:3κ^2^<i>O</i>:<i>O</i>-trihafnium(IV)
Wisniewska, Aleksandra; Baranowska, Katarzyna; Pikies, Jerzy; Acta Crystallographica Section E 64 (2008) m361–m361; doi:10.1107/S1600536807061417

data_2217593
_publ_section_title
Dichlorido-1\k<i>Cl</i>,3\k<i>Cl</i>-hexakis[1,1,2,2,3,3(\h^5^)-methylcyclopentadienyl]di-\m~2~-oxido-1:2\k^2^<i>O</i>:<i>O</i>;2:3\k^2^<i>O</i>:<i>O</i>-trihafnium(IV)
_journal_coeditor_code           NG2389
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m361
_journal_page_last               m361
_journal_paper_doi               10.1107/S1600536807061417
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Hf3 (C6 H7)6 Cl2 O2]'
_chemical_formula_moiety         'C36 H42 Cl2 Hf3 O2'
_chemical_formula_sum            'C36 H42 Cl2 Hf3 O2'
_chemical_formula_weight         1113.07
_chemical_name_systematic
;
Dichlorido-1\kCl,3\kCl-hexakis[1,1,2,2,3,3(\h^5^)-methylcyclopentadienyl]di-
\m~2~-oxido-1:2\k^2^O:O;2:3\k^2^O:O-trihafnium(IV)
;
_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_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 108.466(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9598(10)
_cell_length_b                   12.9710(5)
_cell_length_c                   14.6178(6)
_cell_measurement_reflns_used    6065
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.4265
_cell_measurement_theta_min      1.9305
_cell_volume                     3409.8(3)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_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      120(2)
_diffrn_detector_area_resol_mean 8.1883
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device       '4-axis \k geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction KM4 CCD'
_diffrn_measurement_method       '\w scans, 0.75 deg width'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11353
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    9.298
_exptl_absorpt_correction_T_max  0.434
_exptl_absorpt_correction_T_min  0.283
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.413
_refine_diff_density_min         -2.698
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         5801
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.061
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1162P)^2^+4.6904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1851
_reflns_number_gt                4052
_reflns_number_total             5801
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng2389.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2217593
_cod_database_fobs_code          2217593