#------------------------------------------------------------------------------
#$Date: 2019-11-25 01:59:18 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239914 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/05/4350519.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_4350519
loop_
_publ_author_name
'Milanov, Andrian'
'Bhakta, Raghunandan'
'Baunemann, Arne'
'Becker, Hans-Werner'
'Thomas, Reji'
'Ehrhart, Peter'
'Winter, Manuela'
'Devi, Anjana'
_publ_section_title
;
 Guanidinate-stabilized monomeric hafnium amide complexes as promising
 precursors for MOCVD of HfO2.
;
_journal_issue                   26
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11008
_journal_page_last               11018
_journal_paper_doi               10.1021/ic061056i
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C30 H72 Cl2 Hf2 N18'
_chemical_formula_weight         1112.94
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                100.785(8)
_cell_angle_beta                 112.462(9)
_cell_angle_gamma                110.584(9)
_cell_formula_units_Z            1
_cell_length_a                   10.3253(10)
_cell_length_b                   11.3293(11)
_cell_length_c                   12.1396(12)
_cell_measurement_reflns_used    5343
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.28
_cell_volume                     1140.6(3)
_computing_cell_refinement       'CrysAlis RED 1.171.13, Oxford Diffraction'
_computing_data_collection       'CrysAlis CCD 1.171.13, Oxford Diffraction'
_computing_data_reduction        'CrysAlis RED 1.171.13, Oxford Diffraction'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      104(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Sapphire2-CCD, Oxford Diffraction'
_diffrn_measurement_method       '987 images at 1.0 deg. in ω and 20 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_sigmaI/netI    0.0946
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16290
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    4.708
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_correction_T_min  0.479
_exptl_absorpt_correction_type   'numeric analytical'
_exptl_absorpt_process_details   'Gaussian face-indexed'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.404
_refine_diff_density_min         -1.565
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         5191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0413
_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)+(0.0490P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                4108
_reflns_number_total             5191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061056isi20060613_055714.cif
_cod_data_source_block           cvd55
_cod_original_cell_volume        1140.60(19)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4350519
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 0.52160(3) 0.86248(3) 0.51493(3) 0.01440(10) Uani 1 1 d .
Cl1 Cl 0.76277(19) 0.83428(17) 0.54383(16) 0.0229(4) Uani 1 1 d .
N11 N 0.6465(6) 1.0609(5) 0.5151(5) 0.0138(11) Uani 1 1 d .
C11 C 0.7953(8) 1.1297(6) 0.5455(6) 0.0170(14) Uani 1 1 d .
N12 N 0.8410(6) 1.1666(5) 0.4605(5) 0.0190(12) Uani 1 1 d .
C13 C 0.9757(8) 1.2938(7) 0.4942(7) 0.0252(16) Uani 1 1 d .
H13A H 0.9387 1.3478 0.4484 0.038 Uiso 1 1 calc R
H13B H 1.0487 1.2747 0.4700 0.038 Uiso 1 1 calc R
H13C H 1.0307 1.3445 0.5869 0.038 Uiso 1 1 calc R
C14 C 0.7380(9) 1.0914(7) 0.3243(6) 0.0252(16) Uani 1 1 d .
H14A H 0.6576 1.0030 0.3097 0.038 Uiso 1 1 calc R
H14B H 0.8004 1.0778 0.2841 0.038 Uiso 1 1 calc R
H14C H 0.6859 1.1423 0.2866 0.038 Uiso 1 1 calc R
N15 N 0.9170(6) 1.1721(5) 0.6672(5) 0.0185(12) Uani 1 1 d .
C16 C 1.0668(8) 1.1715(7) 0.6891(7) 0.0260(16) Uani 1 1 d .
H16A H 1.0670 1.1485 0.6072 0.039 Uiso 1 1 calc R
H16B H 1.0780 1.1039 0.7267 0.039 Uiso 1 1 calc R
H16C H 1.1554 1.2616 0.7480 0.039 Uiso 1 1 calc R
C17 C 0.8819(8) 1.1602(7) 0.7707(6) 0.0216(15) Uani 1 1 d .
H17A H 0.7930 1.1793 0.7588 0.032 Uiso 1 1 calc R
H17B H 0.9752 1.2254 0.8530 0.032 Uiso 1 1 calc R
H17C H 0.8537 1.0679 0.7700 0.032 Uiso 1 1 calc R
N21 N 0.3774(6) 0.7009(5) 0.3508(5) 0.0191(12) Uani 1 1 d .
C22 C 0.2967(7) 0.5945(7) 0.2478(6) 0.0183(14) Uani 1 1 d .
N23 N 0.3408(7) 0.5792(6) 0.1515(5) 0.0228(13) Uani 1 1 d .
C23 C 0.2206(9) 0.5335(9) 0.0190(7) 0.039(2) Uani 1 1 d .
H23A H 0.1198 0.4647 0.0045 0.058 Uiso 1 1 calc R
H23B H 0.2531 0.4942 -0.0382 0.058 Uiso 1 1 calc R
H23C H 0.2078 0.6108 0.0013 0.058 Uiso 1 1 calc R
C24 C 0.4920(8) 0.6857(7) 0.1811(7) 0.0236(15) Uani 1 1 d .
H24A H 0.4823 0.7678 0.1765 0.035 Uiso 1 1 calc R
H24B H 0.5236 0.6556 0.1190 0.035 Uiso 1 1 calc R
H24C H 0.5723 0.7055 0.2679 0.035 Uiso 1 1 calc R
N25 N 0.1584(6) 0.4837(5) 0.2175(5) 0.0224(13) Uani 1 1 d .
C26 C 0.1309(9) 0.3457(7) 0.1638(8) 0.0354(19) Uani 1 1 d .
H26A H 0.2033 0.3466 0.1298 0.053 Uiso 1 1 calc R
H26B H 0.0212 0.2899 0.0945 0.053 Uiso 1 1 calc R
H26C H 0.1498 0.3076 0.2311 0.053 Uiso 1 1 calc R
C27 C 0.0887(8) 0.5004(8) 0.2981(7) 0.0314(18) Uani 1 1 d .
H27A H 0.1425 0.4858 0.3764 0.047 Uiso 1 1 calc R
H27B H -0.0240 0.4342 0.2518 0.047 Uiso 1 1 calc R
H27C H 0.1000 0.5925 0.3208 0.047 Uiso 1 1 calc R
N31 N 0.5495(6) 0.8401(5) 0.6810(5) 0.0204(12) Uani 1 1 d .
C31 C 0.5550(7) 0.7965(7) 0.7700(6) 0.0185(14) Uani 1 1 d .
N32 N 0.6149(7) 0.8814(6) 0.8967(5) 0.0232(13) Uani 1 1 d .
C33 C 0.7081(10) 0.8562(8) 1.0052(7) 0.0342(19) Uani 1 1 d .
H33A H 0.6893 0.7620 0.9768 0.051 Uiso 1 1 calc R
H33B H 0.6773 0.8717 1.0714 0.051 Uiso 1 1 calc R
H33C H 0.8208 0.9179 1.0406 0.051 Uiso 1 1 calc R
C34 C 0.6642(9) 1.0247(7) 0.9234(7) 0.0293(17) Uani 1 1 d .
H34A H 0.7779 1.0728 0.9530 0.044 Uiso 1 1 calc R
H34B H 0.6422 1.0612 0.9901 0.044 Uiso 1 1 calc R
H34C H 0.6056 1.0371 0.8450 0.044 Uiso 1 1 calc R
N35 N 0.5019(7) 0.6598(6) 0.7546(5) 0.0236(13) Uani 1 1 d .
C36 C 0.3906(11) 0.6025(8) 0.8003(9) 0.045(2) Uani 1 1 d .
H36A H 0.4092 0.6740 0.8727 0.067 Uiso 1 1 calc R
H36B H 0.4062 0.5304 0.8281 0.067 Uiso 1 1 calc R
H36C H 0.2818 0.5646 0.7306 0.067 Uiso 1 1 calc R
C37 C 0.4632(10) 0.5685(7) 0.6315(7) 0.0353(19) Uani 1 1 d .
H37A H 0.3685 0.5621 0.5629 0.053 Uiso 1 1 calc R
H37B H 0.4431 0.4782 0.6344 0.053 Uiso 1 1 calc R
H37C H 0.5522 0.6041 0.6148 0.053 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N21 Hf1 N31 119.4(2) . .
N21 Hf1 N11 93.6(2) . 2_676
N31 Hf1 N11 98.9(2) . 2_676
N21 Hf1 N11 120.8(2) . .
N31 Hf1 N11 119.8(2) . .
N11 Hf1 N11 77.2(2) 2_676 .
N21 Hf1 Cl1 93.29(16) . .
N31 Hf1 Cl1 90.67(16) . .
N11 Hf1 Cl1 163.46(14) 2_676 .
N11 Hf1 Cl1 86.33(14) . .
N21 Hf1 Hf1 111.70(15) . 2_676
N31 Hf1 Hf1 114.70(16) . 2_676
N11 Hf1 Hf1 38.81(14) 2_676 2_676
N11 Hf1 Hf1 38.42(13) . 2_676
Cl1 Hf1 Hf1 124.73(4) . 2_676
C11 N11 Hf1 126.3(4) . 2_676
C11 N11 Hf1 130.2(4) . .
Hf1 N11 Hf1 102.8(2) 2_676 .
N11 C11 N12 123.1(6) . .
N11 C11 N15 121.9(6) . .
N12 C11 N15 114.9(6) . .
C11 N12 C14 120.2(5) . .
C11 N12 C13 124.2(6) . .
C14 N12 C13 114.6(5) . .
N12 C13 H13A 109.5 . .
N12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
N12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
N12 C14 H14A 109.5 . .
N12 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
N12 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C11 N15 C17 119.5(5) . .
C11 N15 C16 121.5(5) . .
C17 N15 C16 113.5(5) . .
N15 C16 H16A 109.5 . .
N15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
N15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
N15 C17 H17A 109.5 . .
N15 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
N15 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C22 N21 Hf1 174.2(5) . .
N21 C22 N25 124.8(6) . .
N21 C22 N23 122.6(6) . .
N25 C22 N23 112.6(5) . .
C22 N23 C23 118.4(6) . .
C22 N23 C24 115.9(5) . .
C23 N23 C24 112.4(6) . .
N23 C23 H23A 109.5 . .
N23 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
N23 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
N23 C24 H24A 109.5 . .
N23 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
N23 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C22 N25 C27 116.3(5) . .
C22 N25 C26 121.1(5) . .
C27 N25 C26 114.5(6) . .
N25 C26 H26A 109.5 . .
N25 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
N25 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
N25 C27 H27A 109.5 . .
N25 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
N25 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
C31 N31 Hf1 166.2(5) . .
N31 C31 N35 124.4(6) . .
N31 C31 N32 123.2(6) . .
N35 C31 N32 112.4(5) . .
C31 N32 C34 117.7(5) . .
C31 N32 C33 121.0(6) . .
C34 N32 C33 112.5(6) . .
N32 C33 H33A 109.5 . .
N32 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
N32 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
N32 C34 H34A 109.5 . .
N32 C34 H34B 109.5 . .
H34A C34 H34B 109.5 . .
N32 C34 H34C 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
C31 N35 C37 115.3(6) . .
C31 N35 C36 117.8(6) . .
C37 N35 C36 113.5(6) . .
N35 C36 H36A 109.5 . .
N35 C36 H36B 109.5 . .
H36A C36 H36B 109.5 . .
N35 C36 H36C 109.5 . .
H36A C36 H36C 109.5 . .
H36B C36 H36C 109.5 . .
N35 C37 H37A 109.5 . .
N35 C37 H37B 109.5 . .
H37A C37 H37B 109.5 . .
N35 C37 H37C 109.5 . .
H37A C37 H37C 109.5 . .
H37B C37 H37C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hf1 N21 1.997(5) .
Hf1 N31 2.003(5) .
Hf1 N11 2.144(5) 2_676
Hf1 N11 2.162(5) .
Hf1 Cl1 2.5218(16) .
Hf1 Hf1 3.3641(6) 2_676
N11 C11 1.312(8) .
N11 Hf1 2.144(5) 2_676
C11 N12 1.363(8) .
C11 N15 1.373(8) .
N12 C14 1.443(8) .
N12 C13 1.453(8) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
N15 C17 1.451(8) .
N15 C16 1.469(8) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
N21 C22 1.282(8) .
C22 N25 1.385(8) .
C22 N23 1.410(8) .
N23 C23 1.451(9) .
N23 C24 1.452(8) .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C24 H24C 0.9800 .
N25 C27 1.440(9) .
N25 C26 1.454(9) .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
N31 C31 1.259(8) .
C31 N35 1.397(8) .
C31 N32 1.405(8) .
N32 C34 1.448(9) .
N32 C33 1.451(8) .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
C34 H34A 0.9800 .
C34 H34B 0.9800 .
C34 H34C 0.9800 .
N35 C37 1.462(9) .
N35 C36 1.465(10) .
C36 H36A 0.9800 .
C36 H36B 0.9800 .
C36 H36C 0.9800 .
C37 H37A 0.9800 .
C37 H37B 0.9800 .
C37 H37C 0.9800 .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N21 Hf1 N11 C11 -103.1(6) . .
N31 Hf1 N11 C11 77.2(6) . .
N11 Hf1 N11 C11 170.3(7) 2_676 .
Cl1 Hf1 N11 C11 -11.5(5) . .
Hf1 Hf1 N11 C11 170.3(7) 2_676 .
N21 Hf1 N11 Hf1 86.6(3) . 2_676
N31 Hf1 N11 Hf1 -93.1(3) . 2_676
N11 Hf1 N11 Hf1 0.0 2_676 2_676
Cl1 Hf1 N11 Hf1 178.24(17) . 2_676
Hf1 N11 C11 N12 -73.7(7) 2_676 .
Hf1 N11 C11 N12 118.1(6) . .
Hf1 N11 C11 N15 105.1(6) 2_676 .
Hf1 N11 C11 N15 -63.1(8) . .
N11 C11 N12 C14 -23.6(9) . .
N15 C11 N12 C14 157.5(6) . .
N11 C11 N12 C13 144.2(6) . .
N15 C11 N12 C13 -34.7(8) . .
N11 C11 N15 C17 -10.0(9) . .
N12 C11 N15 C17 169.0(5) . .
N11 C11 N15 C16 142.3(6) . .
N12 C11 N15 C16 -38.8(8) . .
N31 Hf1 N21 C22 -85(5) . .
N11 Hf1 N21 C22 173(5) 2_676 .
N11 Hf1 N21 C22 96(5) . .
Cl1 Hf1 N21 C22 8(5) . .
Hf1 Hf1 N21 C22 138(5) 2_676 .
Hf1 N21 C22 N25 122(5) . .
Hf1 N21 C22 N23 -59(5) . .
N21 C22 N23 C23 -132.3(7) . .
N25 C22 N23 C23 47.3(8) . .
N21 C22 N23 C24 5.7(9) . .
N25 C22 N23 C24 -174.7(6) . .
N21 C22 N25 C27 10.6(10) . .
N23 C22 N25 C27 -169.0(6) . .
N21 C22 N25 C26 -136.4(7) . .
N23 C22 N25 C26 44.0(9) . .
N21 Hf1 N31 C31 21(2) . .
N11 Hf1 N31 C31 120(2) 2_676 .
N11 Hf1 N31 C31 -160(2) . .
Cl1 Hf1 N31 C31 -74(2) . .
Hf1 Hf1 N31 C31 157(2) 2_676 .
Hf1 N31 C31 N35 -4(2) . .
Hf1 N31 C31 N32 176.1(17) . .
N31 C31 N32 C34 3.5(10) . .
N35 C31 N32 C34 -176.0(6) . .
N31 C31 N32 C33 -141.6(7) . .
N35 C31 N32 C33 38.9(8) . .
N31 C31 N35 C37 10.5(10) . .
N32 C31 N35 C37 -170.0(6) . .
N31 C31 N35 C36 -127.9(8) . .
N32 C31 N35 C36 51.6(8) . .
