#------------------------------------------------------------------------------
#$Date: 2015-07-03 10:29:35 +0300 (Fri, 03 Jul 2015) $
#$Revision: 139946 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/09/7220992.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_7220992
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         'C38 H54 Cl2 Hf2 N4'
_chemical_formula_sum            'C38 H54 Cl2 Hf2 N4'
_chemical_formula_weight         994.73
_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                112.212(4)
_cell_angle_beta                 102.671(6)
_cell_angle_gamma                104.562(4)
_cell_formula_units_Z            1
_cell_length_a                   9.2969(7)
_cell_length_b                   10.3570(5)
_cell_length_c                   11.6491(5)
_cell_measurement_reflns_used    18255
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     941.17(11)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18182
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.685
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_correction_T_min  0.346
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.562
_refine_diff_density_min         -1.883
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0352P)²+0.7920P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0596
_reflns_number_gt                4076
_reflns_number_total             4300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra07742g2.cif
_cod_data_source_block           10
_cod_database_code               7220992
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 0.100348(13) 0.150634(13) 1.013126(11) 0.01702(6) Uani 1 1 d .
Cl1 Cl 0.37288(9) 0.18472(10) 1.03547(8) 0.02672(17) Uani 1 1 d .
N1 N -0.0359(3) -0.0562(3) 0.8655(3) 0.0199(5) Uani 1 1 d .
C12 C 0.1352(4) 0.3572(4) 0.9462(3) 0.0243(7) Uani 1 1 d .
C19 C -0.2609(4) 0.1940(5) 0.9679(4) 0.0331(8) Uani 1 1 d .
H19A H -0.3212 0.2537 0.9559 0.040 Uiso 1 1 d R
H19B H -0.2643 0.1816 1.0450 0.040 Uiso 1 1 d R
H19C H -0.3052 0.0974 0.8915 0.040 Uiso 1 1 d R
C8 C 0.3661(6) -0.0069(8) 0.6239(5) 0.073(2) Uani 1 1 d .
H8A H 0.4409 0.0252 0.7098 0.088 Uiso 1 1 d R
H8B H 0.3376 0.0754 0.6221 0.088 Uiso 1 1 d R
H8C H 0.4131 -0.0401 0.5580 0.088 Uiso 1 1 d R
C11 C 0.1719(4) 0.4256(4) 1.0845(3) 0.0234(7) Uani 1 1 d .
C15 C 0.0158(5) 0.4276(4) 1.2445(4) 0.0321(8) Uani 1 1 d .
H15A H 0.1044 0.4306 1.3075 0.039 Uiso 1 1 d R
H15B H -0.0807 0.3599 1.2386 0.039 Uiso 1 1 d R
H15C H 0.0123 0.5263 1.2728 0.039 Uiso 1 1 d R
N2 N 0.2229(4) -0.1289(4) 0.5959(3) 0.0379(8) Uani 1 1 d .
C2 C -0.0290(4) -0.1681(4) 0.6404(3) 0.0209(6) Uani 1 1 d .
C1 C -0.1141(4) -0.1485(3) 0.7280(3) 0.0192(6) Uani 1 1 d .
C6 C -0.2791(4) -0.2247(4) 0.6751(3) 0.0228(6) Uani 1 1 d .
H6 H -0.3365 -0.2105 0.7318 0.027 Uiso 1 1 d R
C3 C -0.1101(4) -0.2647(4) 0.5067(3) 0.0284(7) Uani 1 1 d .
H3 H -0.0539 -0.2767 0.4490 0.034 Uiso 1 1 d R
C16 C 0.3320(4) 0.5374(4) 1.1873(4) 0.0329(8) Uani 1 1 d .
H16A H 0.3481 0.6342 1.1905 0.039 Uiso 1 1 d R
H16B H 0.4142 0.5046 1.1645 0.039 Uiso 1 1 d R
H16C H 0.3351 0.5443 1.2724 0.039 Uiso 1 1 d R
C5 C -0.3584(4) -0.3212(4) 0.5412(4) 0.0302(8) Uani 1 1 d .
H5 H -0.4681 -0.3695 0.5085 0.036 Uiso 1 1 d R
C10 C 0.0327(4) 0.3747(4) 1.1109(3) 0.0237(7) Uani 1 1 d .
C13 C -0.0280(4) 0.2619(4) 0.8852(3) 0.0230(6) Uani 1 1 d .
C18 C -0.1216(5) 0.1740(4) 0.7387(4) 0.0325(8) Uani 1 1 d .
H18A H -0.1659 0.2353 0.7095 0.039 Uiso 1 1 d R
H18B H -0.2057 0.0856 0.7215 0.039 Uiso 1 1 d R
H18C H -0.0528 0.1453 0.6918 0.039 Uiso 1 1 d R
C14 C -0.0910(4) 0.2723(4) 0.9874(3) 0.0231(7) Uani 1 1 d .
C17 C 0.2478(5) 0.3848(4) 0.8761(4) 0.0326(8) Uani 1 1 d .
H17A H 0.2126 0.2997 0.7908 0.039 Uiso 1 1 d R
H17B H 0.3513 0.3985 0.9278 0.039 Uiso 1 1 d R
H17C H 0.2524 0.4730 0.8653 0.039 Uiso 1 1 d R
C7 C 0.1471(4) -0.0796(4) 0.6925(3) 0.0288(8) Uani 1 1 d .
H7A H 0.1641 0.0255 0.7197 0.035 Uiso 1 1 d R
H7B H 0.1969 -0.0883 0.7703 0.035 Uiso 1 1 d R
C4 C -0.2730(4) -0.3430(5) 0.4564(3) 0.0330(8) Uani 1 1 d .
H4 H -0.3243 -0.4109 0.3671 0.040 Uiso 1 1 d R
C9 C 0.2577(6) -0.2582(7) 0.5928(5) 0.0591(15) Uani 1 1 d .
H9A H 0.3285 -0.2319 0.6785 0.071 Uiso 1 1 d R
H9B H 0.3072 -0.2888 0.5283 0.071 Uiso 1 1 d R
H9C H 0.1615 -0.3392 0.5696 0.071 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 0.112
1 0 0 0.073
0 -1 0 0.129
0 1 0 0.077
-1 1 0 0.083
0 0 1 0.011
0 0 -1 0.075
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 83.71(11) . 2_557
N1 Hf1 Cl1 107.63(8) . .
N1 Hf1 Cl1 109.13(8) 2_557 .
N1 Hf1 C14 97.75(11) . .
N1 Hf1 C14 102.38(11) 2_557 .
Cl1 Hf1 C14 141.12(8) . .
N1 Hf1 C10 130.34(11) . .
N1 Hf1 C10 96.18(11) 2_557 .
Cl1 Hf1 C10 118.86(8) . .
C14 Hf1 C10 33.55(11) . .
N1 Hf1 C13 89.92(11) . .
N1 Hf1 C13 133.90(11) 2_557 .
Cl1 Hf1 C13 116.27(8) . .
C14 Hf1 C13 33.38(11) . .
C10 Hf1 C13 55.23(11) . .
N1 Hf1 C11 144.59(11) . .
N1 Hf1 C11 121.18(11) 2_557 .
Cl1 Hf1 C11 88.63(8) . .
C14 Hf1 C11 55.10(11) . .
C10 Hf1 C11 33.04(11) . .
C13 Hf1 C11 54.77(11) . .
N1 Hf1 C12 114.95(11) . .
N1 Hf1 C12 150.83(11) 2_557 .
Cl1 Hf1 C12 87.26(8) . .
C14 Hf1 C12 54.99(11) . .
C10 Hf1 C12 54.68(11) . .
C13 Hf1 C12 33.06(11) . .
C11 Hf1 C12 32.66(11) . .
N1 Hf1 Hf1 43.03(7) . 2_557
N1 Hf1 Hf1 40.67(7) 2_557 2_557
Cl1 Hf1 Hf1 115.07(2) . 2_557
C14 Hf1 Hf1 103.63(8) . 2_557
C10 Hf1 Hf1 119.89(8) . 2_557
C13 Hf1 Hf1 118.37(8) . 2_557
C11 Hf1 Hf1 152.86(8) . 2_557
C12 Hf1 Hf1 151.17(8) . 2_557
C1 N1 Hf1 147.4(2) . .
C1 N1 Hf1 115.6(2) . 2_557
Hf1 N1 Hf1 96.29(11) . 2_557
C11 C12 C13 108.2(3) . .
C11 C12 C17 125.6(3) . .
C13 C12 C17 126.2(3) . .
C11 C12 Hf1 73.24(19) . .
C13 C12 Hf1 72.46(18) . .
C17 C12 Hf1 121.8(2) . .
C14 C19 H19A 109.5 . .
C14 C19 H19B 108.8 . .
H19A C19 H19B 109.5 . .
C14 C19 H19C 110.1 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
N2 C8 H8A 110.0 . .
N2 C8 H8B 108.6 . .
H8A C8 H8B 109.5 . .
N2 C8 H8C 109.8 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C12 C11 C10 108.4(3) . .
C12 C11 C16 125.9(3) . .
C10 C11 C16 125.7(3) . .
C12 C11 Hf1 74.11(19) . .
C10 C11 Hf1 72.47(18) . .
C16 C11 Hf1 120.6(2) . .
C10 C15 H15A 109.9 . .
C10 C15 H15B 109.3 . .
H15A C15 H15B 109.5 . .
C10 C15 H15C 109.2 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C9 N2 C7 110.6(3) . .
C9 N2 C8 111.1(4) . .
C7 N2 C8 110.8(4) . .
C3 C2 C1 119.1(3) . .
C3 C2 C7 121.1(3) . .
C1 C2 C7 119.7(3) . .
C6 C1 C2 118.2(3) . .
C6 C1 N1 120.6(3) . .
C2 C1 N1 121.2(3) . .
C5 C6 C1 121.9(3) . .
C5 C6 H6 119.3 . .
C1 C6 H6 118.8 . .
C2 C3 C4 121.9(3) . .
C2 C3 H3 119.0 . .
C4 C3 H3 119.1 . .
C11 C16 H16A 109.6 . .
C11 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C11 C16 H16C 109.3 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C4 C5 C6 119.4(3) . .
C4 C5 H5 120.4 . .
C6 C5 H5 120.1 . .
C11 C10 C14 107.7(3) . .
C11 C10 C15 126.0(3) . .
C14 C10 C15 126.1(3) . .
C11 C10 Hf1 74.49(19) . .
C14 C10 Hf1 72.40(19) . .
C15 C10 Hf1 122.1(2) . .
C14 C13 C12 107.6(3) . .
C14 C13 C18 125.5(3) . .
C12 C13 C18 126.7(3) . .
C14 C13 Hf1 72.06(19) . .
C12 C13 Hf1 74.49(19) . .
C18 C13 Hf1 122.4(2) . .
C13 C18 H18A 109.3 . .
C13 C18 H18B 109.6 . .
H18A C18 H18B 109.5 . .
C13 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C13 C14 C10 108.1(3) . .
C13 C14 C19 125.8(3) . .
C10 C14 C19 126.1(3) . .
C13 C14 Hf1 74.56(19) . .
C10 C14 Hf1 74.05(19) . .
C19 C14 Hf1 119.5(2) . .
C12 C17 H17A 109.4 . .
C12 C17 H17B 108.8 . .
H17A C17 H17B 109.5 . .
C12 C17 H17C 110.2 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
N2 C7 C2 113.3(3) . .
N2 C7 H7A 108.9 . .
C2 C7 H7A 108.7 . .
N2 C7 H7B 109.0 . .
C2 C7 H7B 109.0 . .
H7A C7 H7B 107.7 . .
C5 C4 C3 119.3(3) . .
C5 C4 H4 120.2 . .
C3 C4 H4 120.5 . .
N2 C9 H9A 109.2 . .
N2 C9 H9B 109.2 . .
H9A C9 H9B 109.5 . .
N2 C9 H9C 110.0 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 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 2.012(3) .
Hf1 N1 2.106(3) 2_557
Hf1 Cl1 2.4090(8) .
Hf1 C14 2.454(3) .
Hf1 C10 2.475(3) .
Hf1 C13 2.486(3) .
Hf1 C11 2.501(3) .
Hf1 C12 2.512(3) .
Hf1 Hf1 3.0679(3) 2_557
N1 C1 1.411(4) .
N1 Hf1 2.106(3) 2_557
C12 C11 1.410(5) .
C12 C13 1.422(5) .
C12 C17 1.498(5) .
C19 C14 1.504(5) .
C19 H19A 0.9599 .
C19 H19B 0.9600 .
C19 H19C 0.9601 .
C8 N2 1.459(6) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9601 .
C11 C10 1.415(5) .
C11 C16 1.515(5) .
C15 C10 1.501(5) .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
N2 C9 1.444(7) .
N2 C7 1.456(4) .
C2 C3 1.387(4) .
C2 C1 1.409(4) .
C2 C7 1.509(4) .
C1 C6 1.402(4) .
C6 C5 1.386(5) .
C6 H6 0.9300 .
C3 C4 1.389(5) .
C3 H3 0.9300 .
C16 H16A 0.9600 .
C16 H16B 0.9601 .
C16 H16C 0.9600 .
C5 C4 1.386(5) .
C5 H5 0.9299 .
C10 C14 1.423(5) .
C13 C14 1.419(5) .
C13 C18 1.508(5) .
C18 H18A 0.9599 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C17 H17A 0.9601 .
C17 H17B 0.9601 .
C17 H17C 0.9600 .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C4 H4 0.9300 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
