Crystal structure of bis(pentamethylcyclopentadienyl)-(1-tert-butylisocyanido)-2-trimethylsilyl-3- [(trimethylsilyl)ethynyl]hafnacyclopropene, (C10H15)2(C5H9N)Hf(C10H18Si2)
Torsten Beweries; Anke Spannenberg; Uwe Rosenthal; Zeitschrift für Kristallographie - New Crystal Structures 225 (2010) 191–; doi:

data_8102659
_publ_section_title
;
 Crystal structure of
 bis(pentamethylcyclopentadienyl)-(1-tert-butylisocyanido)-2-trimethylsilyl-3-
 [(trimethylsilyl)ethynyl]hafnacyclopropene,
 (C10H15)2(C5H9N)Hf(C10H18Si2)
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              191
_journal_volume                  225
_journal_year                    2010
_chemical_formula_sum            'C35 H57 Hf N Si2'
_chemical_formula_weight         726.49
_chemical_name_systematic
; 
1,1-Bis(pentamethylcyclopentadienyl)(1-<i>tert</i>-butylisocyanido)
-2-trimethylsilyl-3-[(trimethylsilyl)ethynyl]hafnacyclopropene,
C~35~H~57~HfNSi~2~
;
_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_creation_method           SHELXL-97
_audit_update_record
;
2010-01-25 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.512(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7410(3)
_cell_length_b                   16.2302(5)
_cell_length_c                   21.6945(7)
_cell_measurement_reflns_used    3989
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      1.60
_cell_volume                     3661.3(2)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0594
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            45456
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    2.936
_exptl_absorpt_correction_T_max  0.5849
_exptl_absorpt_correction_T_min  0.3709
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE and X-RED32 (Stoe & Cie, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.101
_refine_diff_density_min         -1.520
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         6682
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0918P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1378
_reflns_number_gt                5021
_reflns_number_total             6682
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2908.cff
_cod_data_source_block           ks744m
_cod_original_cell_volume        3661.31(19)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               8102659