Crystal structure of (1,3-di-<i>tert</i>-butyl-η^5^-cyclopentadienyl)trimethylhafnium(IV)
Pérez-Redondo, Adrián; Varela-Izquierdo, Víctor; Yélamos, Carlos; Acta Crystallographica Section E 71 (2015) m100–m101; doi:10.1107/S205698901500585X

data_2240535
_publ_section_title
;
 Crystal structure of
 (1,3-di-<i>tert</i>-butyl-\h^5^-cyclopentadienyl)trimethylhafnium(IV)
;
_journal_coeditor_code           WM5139
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m100
_journal_page_last               m101
_journal_paper_doi               10.1107/S205698901500585X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Hf (C H3)3 (C13 H21)]'
_chemical_formula_moiety         'C16 H30 Hf'
_chemical_formula_sum            'C16 H30 Hf'
_chemical_formula_weight         400.89
_chemical_name_systematic
;
(1,3-Di-<i>tert</i>-butyl-\h^5^-cyclopentadienyl)trimethylhafnium(IV)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 109.63(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.238(3)
_cell_length_b                   9.613(2)
_cell_length_c                   14.486(3)
_cell_measurement_reflns_used    117
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      3
_cell_volume                     1736.3(7)
_computing_cell_refinement
;
DIRAX (Duisenberg <i>et al.</i>, 2000)
;
_computing_data_collection
;
COLLECT (Nonius, 1998)
;
_computing_data_reduction
;
EvalCCD (Duisenberg <i>et al.</i>, 2003)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
WinGX (Farrugia, 2012) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1001
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29484
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.232
_diffrn_reflns_theta_min         3.268
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.99
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_correction_T_min  0.297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Blessing, 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.415
_refine_diff_density_min         -1.348
_refine_ls_extinction_coef       0.0113(4)
_refine_ls_extinction_method
;
SHELXL-2014/7 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3136
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+1.4700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.073
_reflns_number_gt                2471
_reflns_number_total             3136
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5139sup1.cif
_cod_data_source_block           I
_cod_database_code               2240535
_cod_database_fobs_code          2240535