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#$Date: 2016-03-22 11:08:12 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178886 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/15/4111506.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4111506
loop_
_publ_author_name
'Holger Braunschweig'
'Manuela Gross'
'Mario Kraft'
'Marc O. Kristen'
'Dirk Leusser'
_publ_contact_author             'Prof. Dr. Holger Braunschweig'
_publ_contact_author_email       h.braunschweig@mail.uni-wuerzburg.de
_publ_section_title
;
 [2]Borametallocenophanes of Zr and Hf: Synthesis, Structure, and
 Polymerization Activity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3282
_journal_page_last               3283
_journal_paper_doi               10.1021/ja042408s
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C14 H20 B2 Cl2 Hf N2'
_chemical_formula_weight         487.33
_chemical_name_systematic
; 
 ? 
;
_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                 104.7240(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7775(8)
_cell_length_b                   12.1721(10)
_cell_length_c                   14.8995(12)
_cell_measurement_reflns_used    8598
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.25
_cell_volume                     1715.0(2)
_computing_cell_refinement       'SAINT-NT V5/6.0'
_computing_data_collection       'SMART-NT V5.6'
_computing_data_reduction        'SAINT-NT V5/6.0'
_computing_molecular_graphics    'SHELXTL-NT V5.1'
_computing_publication_material  'SHELXTL-NT V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Smart Apex with D8-Goniometer'
_diffrn_measurement_method       'omega scan'
_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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            33417
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    6.386
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS 2.05; Sheldrick'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_description       plate
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.198
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0202
_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/[σ²(Fo²)+(0.0330P)²+0.4104P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0518
_reflns_number_gt                3556
_reflns_number_total             3919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja042408ssi20041230_081309.cif
_cod_data_source_block           MG08
_cod_database_code               4111506
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Hf1 Hf 0.767148(11) 0.149352(8) 0.240194(7) 0.02190(5) Uani 1 1 d .
Cl2 Cl 0.87433(7) 0.00319(5) 0.17058(5) 0.03235(15) Uani 1 1 d .
Cl1 Cl 0.90444(8) 0.29764(5) 0.19617(5) 0.03350(15) Uani 1 1 d .
C5 C 0.7310(3) 0.1638(2) 0.40034(18) 0.0247(5) Uani 1 1 d .
C3 C 0.9605(3) 0.1693(3) 0.3866(2) 0.0337(7) Uani 1 1 d .
H3 H 1.0499 0.1964 0.3827 0.040 Uiso 1 1 calc R
C7 C 0.5057(3) 0.1391(2) 0.2205(2) 0.0259(6) Uani 1 1 d .
C6 C 0.5375(3) 0.0653(2) 0.15501(19) 0.0308(6) Uani 1 1 d .
H6 H 0.5285 -0.0124 0.1563 0.037 Uiso 1 1 calc R
C10 C 0.5849(3) 0.1256(3) 0.0872(2) 0.0351(7) Uani 1 1 d .
H10 H 0.6125 0.0956 0.0356 0.042 Uiso 1 1 calc R
C1 C 0.7772(3) 0.0545(2) 0.38731(17) 0.0272(5) Uani 1 1 d .
H1 H 0.7212 -0.0101 0.3826 0.033 Uiso 1 1 calc R
C2 C 0.9201(3) 0.0586(3) 0.38268(19) 0.0318(6) Uani 1 1 d .
H2 H 0.9780 -0.0027 0.3778 0.038 Uiso 1 1 calc R
C9 C 0.5841(3) 0.2370(3) 0.10971(19) 0.0346(7) Uani 1 1 d .
H9 H 0.6086 0.2962 0.0752 0.042 Uiso 1 1 calc R
C4 C 0.8458(3) 0.2336(2) 0.39746(18) 0.0295(6) Uani 1 1 d .
H4 H 0.8455 0.3114 0.4021 0.035 Uiso 1 1 calc R
C8 C 0.5402(3) 0.2462(2) 0.19279(18) 0.0290(6) Uani 1 1 d .
H8 H 0.5344 0.3127 0.2251 0.035 Uiso 1 1 calc R
N1 N 0.3602(2) 0.0423(2) 0.32179(17) 0.0333(5) Uani 1 1 d .
N2 N 0.5407(3) 0.26904(19) 0.46067(15) 0.0321(5) Uani 1 1 d .
C20 C 0.2770(3) -0.0242(3) 0.2458(2) 0.0449(8) Uani 1 1 d .
H20A H 0.2955 -0.0003 0.1872 0.067 Uiso 1 1 calc R
H20B H 0.1762 -0.0153 0.2425 0.067 Uiso 1 1 calc R
H20C H 0.3033 -0.1016 0.2568 0.067 Uiso 1 1 calc R
C22 C 0.6439(4) 0.3269(3) 0.5342(2) 0.0411(8) Uani 1 1 d .
H22A H 0.7374 0.2935 0.5419 0.062 Uiso 1 1 calc R
H22B H 0.6155 0.3213 0.5925 0.062 Uiso 1 1 calc R
H22C H 0.6477 0.4044 0.5172 0.062 Uiso 1 1 calc R
B1 B 0.5727(3) 0.1913(3) 0.4015(2) 0.0271(6) Uani 1 1 d .
B2 B 0.4621(3) 0.1189(3) 0.3145(2) 0.0282(6) Uani 1 1 d .
C21 C 0.3282(3) 0.0162(3) 0.4099(2) 0.0460(8) Uani 1 1 d .
H21A H 0.3867 0.0617 0.4593 0.069 Uiso 1 1 calc R
H21B H 0.3482 -0.0616 0.4245 0.069 Uiso 1 1 calc R
H21C H 0.2280 0.0309 0.4051 0.069 Uiso 1 1 calc R
C23 C 0.3960(4) 0.3047(3) 0.4543(2) 0.0470(8) Uani 1 1 d .
H23A H 0.3318 0.2695 0.4007 0.071 Uiso 1 1 calc R
H23B H 0.3899 0.3847 0.4468 0.071 Uiso 1 1 calc R
H23C H 0.3693 0.2839 0.5110 0.071 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
Cl2 Hf1 Cl1 95.78(3)
Cl2 Hf1 C7 116.91(6)
Cl1 Hf1 C7 128.45(6)
Cl2 Hf1 C5 129.71(6)
Cl1 Hf1 C5 115.16(6)
C7 Hf1 C5 74.23(9)
C4 C5 C1 105.9(2)
C4 C5 B1 131.0(2)
C1 C5 B1 122.6(2)
C4 C5 Hf1 73.06(15)
C1 C5 Hf1 71.38(14)
B1 C5 Hf1 113.53(16)
C2 C3 C4 108.3(3)
C6 C7 C8 105.7(3)
C6 C7 B2 131.7(2)
C8 C7 B2 122.1(2)
C6 C7 Hf1 73.53(16)
C8 C7 Hf1 71.37(15)
B2 C7 Hf1 113.61(17)
C7 C6 C10 109.3(3)
C9 C10 C6 108.0(3)
C2 C1 C5 108.8(2)
C3 C2 C1 107.6(3)
C10 C9 C8 108.0(3)
C3 C4 C5 109.3(3)
C9 C8 C7 109.0(3)
B2 N1 C20 125.5(3)
B2 N1 C21 122.6(3)
C20 N1 C21 111.8(2)
B1 N2 C23 122.3(3)
B1 N2 C22 125.5(3)
C23 N2 C22 112.2(3)
N2 B1 C5 122.1(3)
N2 B1 B2 129.5(3)
C5 B1 B2 108.2(2)
N1 B2 C7 122.2(3)
N1 B2 B1 128.0(3)
C7 B2 B1 109.3(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Hf1 Cl2 2.4272(7)
Hf1 Cl1 2.4367(7)
Hf1 C7 2.501(3)
Hf1 C5 2.505(3)
C5 C4 1.417(4)
C5 C1 1.433(4)
C5 B1 1.589(4)
C3 C2 1.402(4)
C3 C4 1.409(4)
C7 C6 1.417(4)
C7 C8 1.433(4)
C7 B2 1.584(4)
C6 C10 1.419(4)
C10 C9 1.397(4)
C1 C2 1.417(4)
C9 C8 1.414(4)
N1 B2 1.388(4)
N1 C20 1.460(4)
N1 C21 1.461(4)
N2 B1 1.382(4)
N2 C23 1.459(4)
N2 C22 1.467(4)
B1 B2 1.707(5)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
Cl2 Hf1 C5 C4 104.27(16)
Cl1 Hf1 C5 C4 -18.05(18)
C7 Hf1 C5 C4 -143.59(17)
Cl2 Hf1 C5 C1 -9.57(18)
Cl1 Hf1 C5 C1 -131.89(14)
C7 Hf1 C5 C1 102.57(16)
Cl2 Hf1 C5 B1 -127.80(16)
Cl1 Hf1 C5 B1 109.88(17)
C7 Hf1 C5 B1 -15.66(18)
Cl2 Hf1 C7 C6 -15.44(18)
Cl1 Hf1 C7 C6 107.74(16)
C5 Hf1 C7 C6 -142.39(18)
Cl2 Hf1 C7 C8 -128.85(14)
Cl1 Hf1 C7 C8 -5.68(19)
C5 Hf1 C7 C8 104.19(17)
Cl2 Hf1 C7 B2 113.47(18)
Cl1 Hf1 C7 B2 -123.36(17)
C5 Hf1 C7 B2 -13.49(18)
C8 C7 C6 C10 -2.1(3)
B2 C7 C6 C10 -173.9(3)
Hf1 C7 C6 C10 -66.7(2)
C7 C6 C10 C9 0.3(3)
C4 C5 C1 C2 3.6(3)
B1 C5 C1 C2 175.6(2)
Hf1 C5 C1 C2 69.08(18)
C4 C3 C2 C1 2.3(3)
C5 C1 C2 C3 -3.7(3)
C6 C10 C9 C8 1.7(3)
C2 C3 C4 C5 -0.1(3)
C1 C5 C4 C3 -2.2(3)
B1 C5 C4 C3 -173.2(3)
Hf1 C5 C4 C3 -66.48(19)
C10 C9 C8 C7 -3.0(3)
C6 C7 C8 C9 3.2(3)
B2 C7 C8 C9 175.9(2)
Hf1 C7 C8 C9 69.23(19)
C23 N2 B1 C5 172.1(3)
C22 N2 B1 C5 -6.3(4)
C23 N2 B1 B2 -1.9(4)
C22 N2 B1 B2 179.7(3)
C4 C5 B1 N2 -47.8(4)
C1 C5 B1 N2 142.4(3)
Hf1 C5 B1 N2 -135.3(2)
C4 C5 B1 B2 127.3(3)
C1 C5 B1 B2 -42.5(3)
Hf1 C5 B1 B2 39.8(3)
C20 N1 B2 C7 -3.0(4)
C21 N1 B2 C7 174.5(3)
C20 N1 B2 B1 -174.4(3)
C21 N1 B2 B1 3.1(4)
C6 C7 B2 N1 -45.9(4)
C8 C7 B2 N1 143.4(3)
Hf1 C7 B2 N1 -134.5(2)
C6 C7 B2 B1 126.9(3)
C8 C7 B2 B1 -43.8(3)
Hf1 C7 B2 B1 38.3(3)
N2 B1 B2 N1 -64.2(4)
C5 B1 B2 N1 121.2(3)
N2 B1 B2 C7 123.5(3)
C5 B1 B2 C7 -51.1(3)
