Crystal structure of bis(pentamethylcyclopentadienyl)-(4,4'-di-tert-butylbipyridyl)hafnium(IV) — hexane (1:0.5), Hf(C10H15)2(C18H24N2) · 0.5C6H14
Torsten Beweries; Anke Spannenberg; Uwe Rosenthal; Zeitschrift für Kristallographie - New Crystal Structures 225 (2010) 188–; doi:

data_8102657
_publ_section_title
;
 Crystal structure of
 bis(pentamethylcyclopentadienyl)-(4,4'-di-tert-butylbipyridyl)hafnium(IV)
 --- hexane (1:0.5), Hf(C10H15)2(C18H24N2) &#x00B7; 0.5C6H14
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              188
_journal_volume                  225
_journal_year                    2010
_chemical_formula_sum            'C41 H61 Hf N2'
_chemical_formula_weight         760.41
_chemical_name_systematic
; 
1,1-Bis(pentamethylcyclopentadienyl)-(4,4'-di-<i>tert</i>-butyl-bipyridyl)-
hafnium(IV) hexane solvate, C~38~H~54~HfN~2~ . 0.5C~6~H~14~

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.144(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4410(4)
_cell_length_b                   13.9983(6)
_cell_length_c                   21.1996(8)
_cell_measurement_reflns_used    5338
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.21
_cell_measurement_theta_min      1.50
_cell_volume                     3948.5(3)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics    'XP in SHELXTL'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'STOE IPDS II'
_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  0.1109
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55798
_diffrn_reflns_theta_full        26.80
_diffrn_reflns_theta_max         26.80
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    2.669
_exptl_absorpt_correction_T_max  0.6069
_exptl_absorpt_correction_T_min  0.3206
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE and X-RED32 (Stoe & Cie, 2005)'
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.198
_refine_diff_density_min         -2.243
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         8368
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1206
_reflns_number_gt                6265
_reflns_number_total             8368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2904.cff
_cod_data_source_block           ks676
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               8102657