#------------------------------------------------------------------------------
#$Date: 2015-07-03 10:29:35 +0300 (Fri, 03 Jul 2015) $
#$Revision: 139946 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/09/7220995.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_7220995
loop_
_publ_author_name
'Havlik, Ales'
'Lamač, Martin'
'Pinkas, Jiri'
'R°užička, Aleš'
'Horacek, Michal'
_publ_section_title
;
 Mixed Amido-cyclopentadienyl Group 4 Metal Complexes
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA07742G
_journal_year                    2015
_chemical_formula_moiety         'C42 H60 Cl2 Hf2 N2'
_chemical_formula_sum            'C42 H60 Cl2 Hf2 N2'
_chemical_formula_weight         1020.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-06-22 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                113.815(5)
_cell_angle_beta                 103.680(4)
_cell_angle_gamma                98.356(5)
_cell_formula_units_Z            1
_cell_length_a                   10.1859(5)
_cell_length_b                   10.5241(9)
_cell_length_c                   10.6120(7)
_cell_measurement_reflns_used    20069
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     973.38(13)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_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  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19985
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.14
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.498
_exptl_absorpt_correction_T_max  0.764
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.763
_refine_diff_density_min         -2.064
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0260
_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)+(0.0390P)²+1.0782P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0651
_reflns_number_gt                4166
_reflns_number_total             4456
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra07742g2.cif
_cod_data_source_block           13
_cod_database_code               7220995
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.381583(13) 0.019147(14) 0.397465(14) 0.01304(6) Uani 1 1 d .
Cl1 Cl 0.39195(9) -0.07379(10) 0.15487(9) 0.02173(18) Uani 1 1 d .
C5 C 0.8716(4) 0.4773(4) 0.7793(4) 0.0215(8) Uani 1 1 d .
H5 H 0.9037 0.5507 0.8745 0.026 Uiso 1 1 d R
N1 N 0.5778(3) 0.1383(3) 0.5342(3) 0.0135(5) Uani 1 1 d .
C16 C 0.1855(4) 0.1070(4) 0.2911(4) 0.0195(7) Uani 1 1 d .
C7 C 0.7167(4) 0.1630(4) 0.3300(4) 0.0190(7) Uani 1 1 d .
H7 H 0.6558 0.0740 0.3161 0.023 Uiso 1 1 d R
C9 C 0.6255(4) 0.2320(4) 0.2541(4) 0.0261(8) Uani 1 1 d .
H9A H 0.5539 0.2547 0.2974 0.031 Uiso 1 1 d R
H9B H 0.5826 0.1655 0.1525 0.031 Uiso 1 1 d R
H9C H 0.6831 0.3187 0.2645 0.031 Uiso 1 1 d R
C17 C 0.1220(4) -0.0212(4) 0.2943(4) 0.0191(7) Uani 1 1 d .
C15 C 0.2555(4) 0.2142(4) 0.4379(4) 0.0201(7) Uani 1 1 d .
C14 C 0.2365(4) 0.1531(4) 0.5321(4) 0.0188(7) Uani 1 1 d .
C1 C 0.6963(3) 0.2598(4) 0.5864(4) 0.0151(7) Uani 1 1 d .
C13 C 0.1543(4) 0.0081(4) 0.4420(4) 0.0196(7) Uani 1 1 d .
H13 H 0.1261 -0.0573 0.4751 0.023 Uiso 1 1 d R
C3 C 0.9010(4) 0.3687(4) 0.5470(4) 0.0220(8) Uani 1 1 d .
H3 H 0.9530 0.3681 0.4857 0.026 Uiso 1 1 d R
C8 C 0.8270(5) 0.1228(5) 0.2575(5) 0.0296(9) Uani 1 1 d .
H8A H 0.8752 0.2043 0.2512 0.036 Uiso 1 1 d R
H8B H 0.7818 0.0444 0.1613 0.036 Uiso 1 1 d R
H8C H 0.8932 0.0939 0.3139 0.036 Uiso 1 1 d R
C6 C 0.7433(4) 0.3739(4) 0.7309(4) 0.0172(7) Uani 1 1 d .
C2 C 0.7742(4) 0.2649(4) 0.4923(4) 0.0175(7) Uani 1 1 d .
C10 C 0.6606(4) 0.3986(4) 0.8367(4) 0.0191(7) Uani 1 1 d .
H10 H 0.5803 0.3139 0.7962 0.023 Uiso 1 1 d R
C21 C 0.0325(4) -0.1604(4) 0.1635(4) 0.0239(8) Uani 1 1 d .
H21A H 0.0340 -0.2388 0.1879 0.029 Uiso 1 1 d R
H21B H 0.0687 -0.1767 0.0842 0.029 Uiso 1 1 d R
H21C H -0.0622 -0.1543 0.1353 0.029 Uiso 1 1 d R
C11 C 0.7479(4) 0.4222(4) 0.9872(4) 0.0241(8) Uani 1 1 d .
H11A H 0.8018 0.3531 0.9759 0.029 Uiso 1 1 d R
H11B H 0.6869 0.4105 1.0406 0.029 Uiso 1 1 d R
H11C H 0.8101 0.5180 1.0396 0.029 Uiso 1 1 d R
C4 C 0.9515(4) 0.4735(4) 0.6912(5) 0.0264(8) Uani 1 1 d .
H4 H 1.0385 0.5401 0.7274 0.032 Uiso 1 1 d R
C12 C 0.6052(4) 0.5309(4) 0.8552(5) 0.0278(9) Uani 1 1 d .
H12A H 0.6830 0.6153 0.8986 0.033 Uiso 1 1 d R
H12B H 0.5480 0.5426 0.9170 0.033 Uiso 1 1 d R
H12C H 0.5502 0.5177 0.7617 0.033 Uiso 1 1 d R
C20 C 0.1707(5) 0.1295(5) 0.1572(5) 0.0289(9) Uani 1 1 d .
H20A H 0.1392 0.0376 0.0720 0.035 Uiso 1 1 d R
H20B H 0.2600 0.1815 0.1645 0.035 Uiso 1 1 d R
H20C H 0.1037 0.1838 0.1500 0.035 Uiso 1 1 d R
C19 C 0.3289(5) 0.3675(4) 0.4827(5) 0.0280(9) Uani 1 1 d .
H19A H 0.3188 0.4298 0.5732 0.034 Uiso 1 1 d R
H19B H 0.2877 0.3940 0.4089 0.034 Uiso 1 1 d R
H19C H 0.4268 0.3770 0.4943 0.034 Uiso 1 1 d R
C18 C 0.2759(4) 0.2308(5) 0.6945(4) 0.0285(9) Uani 1 1 d .
H18A H 0.3546 0.3134 0.7327 0.034 Uiso 1 1 d R
H18B H 0.3004 0.1672 0.7348 0.034 Uiso 1 1 d R
H18C H 0.1976 0.2616 0.7201 0.034 Uiso 1 1 d 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'
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.056
1 0 0 0.025
0 0 1 0.053
0 0 -1 0.012
0 -1 0 0.020
0 1 0 0.065
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Hf1 N1 85.65(11) . 2_656
N1 Hf1 Cl1 107.14(8) . .
N1 Hf1 Cl1 105.14(8) 2_656 .
N1 Hf1 C13 130.32(12) . .
N1 Hf1 C13 92.98(11) 2_656 .
Cl1 Hf1 C13 120.92(9) . .
N1 Hf1 C14 101.11(12) . .
N1 Hf1 C14 108.80(11) 2_656 .
Cl1 Hf1 C14 136.97(9) . .
C13 Hf1 C14 33.30(12) . .
N1 Hf1 C17 154.08(12) . .
N1 Hf1 C17 110.31(11) 2_656 .
Cl1 Hf1 C17 88.78(9) . .
C13 Hf1 C17 32.97(13) . .
C14 Hf1 C17 55.07(12) . .
N1 Hf1 C15 100.30(12) . .
N1 Hf1 C15 141.78(12) 2_656 .
Cl1 Hf1 C15 108.87(9) . .
C13 Hf1 C15 54.49(12) . .
C14 Hf1 C15 32.98(12) . .
C17 Hf1 C15 54.45(12) . .
N1 Hf1 C16 127.48(12) . .
N1 Hf1 C16 143.06(11) 2_656 .
Cl1 Hf1 C16 82.24(9) . .
C13 Hf1 C16 54.44(12) . .
C14 Hf1 C16 54.76(12) . .
C17 Hf1 C16 32.82(12) . .
C15 Hf1 C16 32.71(12) . .
N1 Hf1 Hf1 43.97(8) . 2_656
N1 Hf1 Hf1 41.68(8) 2_656 2_656
Cl1 Hf1 Hf1 112.24(2) . 2_656
C13 Hf1 Hf1 117.89(9) . 2_656
C14 Hf1 Hf1 110.66(9) . 2_656
C17 Hf1 Hf1 147.30(9) . 2_656
C15 Hf1 Hf1 131.78(9) . 2_656
C16 Hf1 Hf1 164.22(9) . 2_656
C4 C5 C6 122.3(4) . .
C4 C5 H5 118.8 . .
C6 C5 H5 118.9 . .
C1 N1 Hf1 150.2(2) . .
C1 N1 Hf1 114.7(2) . 2_656
Hf1 N1 Hf1 94.35(11) . 2_656
C15 C16 C17 107.7(3) . .
C15 C16 C20 125.9(3) . .
C17 C16 C20 126.2(4) . .
C15 C16 Hf1 73.1(2) . .
C17 C16 Hf1 72.6(2) . .
C20 C16 Hf1 124.0(3) . .
C2 C7 C8 115.2(3) . .
C2 C7 C9 108.4(3) . .
C8 C7 C9 109.4(3) . .
C2 C7 H7 107.8 . .
C8 C7 H7 108.0 . .
C9 C7 H7 107.8 . .
C7 C9 H9A 109.7 . .
C7 C9 H9B 109.3 . .
H9A C9 H9B 109.5 . .
C7 C9 H9C 109.4 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C13 C17 C16 107.5(3) . .
C13 C17 C21 126.6(3) . .
C16 C17 C21 125.9(4) . .
C13 C17 Hf1 71.81(19) . .
C16 C17 Hf1 74.6(2) . .
C21 C17 Hf1 120.9(2) . .
C14 C15 C16 108.5(3) . .
C14 C15 C19 126.7(4) . .
C16 C15 C19 124.7(4) . .
C14 C15 Hf1 72.2(2) . .
C16 C15 Hf1 74.2(2) . .
C19 C15 Hf1 122.4(3) . .
C13 C14 C15 106.9(3) . .
C13 C14 C18 125.5(4) . .
C15 C14 C18 127.0(4) . .
C13 C14 Hf1 72.5(2) . .
C15 C14 Hf1 74.8(2) . .
C18 C14 Hf1 124.8(3) . .
C6 C1 C2 118.0(3) . .
C6 C1 N1 122.7(3) . .
C2 C1 N1 119.3(3) . .
C17 C13 C14 109.3(3) . .
C17 C13 Hf1 75.2(2) . .
C14 C13 Hf1 74.2(2) . .
C17 C13 H13 125.4 . .
C14 C13 H13 125.3 . .
Hf1 C13 H13 117.2 . .
C4 C3 C2 121.3(4) . .
C4 C3 H3 119.4 . .
C2 C3 H3 119.3 . .
C7 C8 H8A 109.7 . .
C7 C8 H8B 109.2 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C5 C6 C1 118.8(3) . .
C5 C6 C10 116.4(3) . .
C1 C6 C10 124.7(3) . .
C3 C2 C1 120.1(3) . .
C3 C2 C7 118.8(3) . .
C1 C2 C7 121.0(3) . .
C6 C10 C11 113.0(3) . .
C6 C10 C12 109.7(3) . .
C11 C10 C12 108.5(3) . .
C6 C10 H10 108.7 . .
C11 C10 H10 108.4 . .
C12 C10 H10 108.5 . .
C17 C21 H21A 109.4 . .
C17 C21 H21B 109.6 . .
H21A C21 H21B 109.5 . .
C17 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C10 C11 H11A 109.3 . .
C10 C11 H11B 109.8 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.3 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C5 C4 C3 119.1(3) . .
C5 C4 H4 120.6 . .
C3 C4 H4 120.3 . .
C10 C12 H12A 109.3 . .
C10 C12 H12B 109.6 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C16 C20 H20A 109.6 . .
C16 C20 H20B 109.3 . .
H20A C20 H20B 109.5 . .
C16 C20 H20C 109.6 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C15 C19 H19A 109.4 . .
C15 C19 H19B 109.2 . .
H19A C19 H19B 109.5 . .
C15 C19 H19C 109.8 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C14 C18 H18A 109.6 . .
C14 C18 H18B 109.6 . .
H18A C18 H18B 109.5 . .
C14 C18 H18C 109.2 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hf1 N1 2.026(3) .
Hf1 N1 2.115(3) 2_656
Hf1 Cl1 2.3918(9) .
Hf1 C13 2.466(3) .
Hf1 C14 2.488(4) .
Hf1 C17 2.509(3) .
Hf1 C15 2.522(4) .
Hf1 C16 2.536(4) .
Hf1 Hf1 3.0373(3) 2_656
C5 C4 1.370(6) .
C5 C6 1.405(5) .
C5 H5 0.9300 .
N1 C1 1.435(4) .
N1 Hf1 2.115(3) 2_656
C16 C15 1.424(5) .
C16 C17 1.426(5) .
C16 C20 1.510(6) .
C7 C2 1.519(5) .
C7 C8 1.522(5) .
C7 C9 1.533(5) .
C7 H7 0.9800 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9601 .
C17 C13 1.412(5) .
C17 C21 1.509(5) .
C15 C14 1.423(5) .
C15 C19 1.500(5) .
C14 C13 1.420(5) .
C14 C18 1.496(5) .
C1 C6 1.422(5) .
C1 C2 1.427(5) .
C13 H13 0.9300 .
C3 C4 1.386(6) .
C3 C2 1.386(5) .
C3 H3 0.9299 .
C8 H8A 0.9600 .
C8 H8B 0.9599 .
C8 H8C 0.9600 .
C6 C10 1.520(5) .
C10 C11 1.532(5) .
C10 C12 1.535(5) .
C10 H10 0.9800 .
C21 H21A 0.9601 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C4 H4 0.9300 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C18 H18A 0.9600 .
C18 H18B 0.9599 .
C18 H18C 0.9601 .
