#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:58:00 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178542 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/48/4064844.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_4064844
loop_
_publ_author_name
'Szuromi, Endre'
'Klosin, Jerzy'
'Abboud, Khalil A.'
_publ_section_title
;
 Aminotroponiminato Hafnium and Zirconium Complexes: Synthesis and
 Ethylene/1-Octene Copolymerization Study
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4589
_journal_paper_doi               10.1021/om200362v
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C42 H54 N4'
_chemical_formula_weight         614.89
_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
; 
2008-08-30 # Formatted by publCIF 
;
_cell_angle_alpha                93.799(3)
_cell_angle_beta                 92.376(3)
_cell_angle_gamma                112.706(3)
_cell_formula_units_Z            1
_cell_length_a                   8.1698(14)
_cell_length_b                   8.2525(14)
_cell_length_c                   14.122(3)
_cell_measurement_reflns_used    52
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     874.1(3)
_computing_cell_refinement
'Bruker SMART v5.624 & SAINT 6.36a (Bruker 1998)'
_computing_data_collection       'Bruker SMART v5.624 (Bruker 1998)'
_computing_data_reduction        'Bruker SHELXTL v6.14 (Bruker 2000)'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement  'Bruker SHELXTL v6.14'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'SMART CCD area detector'
_diffrn_measurement_method       '\\w scans'
_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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4879
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.9939
_exptl_absorpt_correction_T_min  0.9899
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.12 (Bruker 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             334
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0426P)²+1.5869P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1854
_refine_ls_wR_factor_ref         0.1912
_reflns_number_gt                2439
_reflns_number_total             3011
_reflns_threshold_expression     I>2\\s(I)
_cod_data_source_file            om200362v_si_002.cif
_cod_data_source_block           19
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064844
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
N1 N 0.1585(3) 0.5493(3) 0.27430(17) 0.0259(6) Uani 1 1 d .
N2 N 0.2005(4) 0.7329(3) 0.43085(18) 0.0286(6) Uani 1 1 d .
H2 H 0.283(5) 0.705(5) 0.397(3) 0.039(10) Uiso 1 1 d .
C1 C 0.0106(4) 0.5592(4) 0.2999(2) 0.0247(7) Uani 1 1 d .
C2 C -0.1534(4) 0.4865(5) 0.2419(2) 0.0336(8) Uani 1 1 d .
H2A H -0.1439 0.4350 0.1812 0.040 Uiso 1 1 calc R
C3 C -0.3201(4) 0.4769(5) 0.2568(3) 0.0415(9) Uani 1 1 d .
H3A H -0.4053 0.4250 0.2043 0.050 Uiso 1 1 calc R
C4 C -0.3865(5) 0.5320(5) 0.3381(3) 0.0430(9) Uani 1 1 d .
H4A H -0.5096 0.5104 0.3348 0.052 Uiso 1 1 calc R
C5 C -0.2896(5) 0.6133(5) 0.4208(3) 0.0385(8) Uani 1 1 d .
H5A H -0.3565 0.6357 0.4697 0.046 Uiso 1 1 calc R
C6 C -0.1068(4) 0.6693(4) 0.4456(2) 0.0313(7) Uani 1 1 d .
H6A H -0.0706 0.7257 0.5081 0.038 Uiso 1 1 calc R
C7 C 0.0300(4) 0.6572(4) 0.3951(2) 0.0257(7) Uani 1 1 d .
C8 C 0.1660(4) 0.4515(4) 0.1890(2) 0.0259(7) Uani 1 1 d .
C9 C 0.2268(4) 0.5399(4) 0.1071(2) 0.0286(7) Uani 1 1 d .
C10 C 0.2540(5) 0.4460(5) 0.0285(2) 0.0362(8) Uani 1 1 d .
H10A H 0.2963 0.5045 -0.0267 0.043 Uiso 1 1 calc R
C11 C 0.2203(5) 0.2674(5) 0.0292(2) 0.0410(9) Uani 1 1 d .
H11A H 0.2409 0.2051 -0.0249 0.049 Uiso 1 1 calc R
C12 C 0.1569(5) 0.1811(5) 0.1085(2) 0.0362(8) Uani 1 1 d .
H12A H 0.1315 0.0586 0.1078 0.043 Uiso 1 1 calc R
C13 C 0.1292(4) 0.2705(4) 0.1900(2) 0.0290(7) Uani 1 1 d .
C14 C 0.2645(4) 0.7364(4) 0.1077(2) 0.0322(8) Uani 1 1 d .
H14A H 0.1682 0.7579 0.1411 0.039 Uiso 1 1 calc R
C15 C 0.2640(5) 0.7969(5) 0.0081(2) 0.0401(9) Uani 1 1 d .
H15A H 0.1504 0.7253 -0.0274 0.060 Uiso 1 1 calc R
H15B H 0.3615 0.7833 -0.0251 0.060 Uiso 1 1 calc R
H15C H 0.2797 0.9212 0.0127 0.060 Uiso 1 1 calc R
C16 C 0.4400(5) 0.8460(5) 0.1633(3) 0.0441(9) Uani 1 1 d .
H16A H 0.4373 0.8096 0.2281 0.066 Uiso 1 1 calc R
H16B H 0.4590 0.9710 0.1659 0.066 Uiso 1 1 calc R
H16C H 0.5372 0.8282 0.1318 0.066 Uiso 1 1 calc R
C17 C 0.0596(5) 0.1705(4) 0.2757(2) 0.0333(8) Uani 1 1 d .
H17A H 0.0477 0.2556 0.3260 0.040 Uiso 1 1 calc R
C18 C 0.1874(5) 0.0962(5) 0.3160(3) 0.0500(10) Uani 1 1 d .
H18A H 0.3049 0.1914 0.3303 0.075 Uiso 1 1 calc R
H18B H 0.1963 0.0071 0.2693 0.075 Uiso 1 1 calc R
H18C H 0.1439 0.0418 0.3745 0.075 Uiso 1 1 calc R
C19 C -0.1225(5) 0.0241(6) 0.2527(3) 0.0537(11) Uani 1 1 d .
H19A H -0.2057 0.0739 0.2288 0.081 Uiso 1 1 calc R
H19B H -0.1651 -0.0340 0.3103 0.081 Uiso 1 1 calc R
H19C H -0.1143 -0.0623 0.2040 0.081 Uiso 1 1 calc R
C20 C 0.2606(4) 0.8361(5) 0.5227(2) 0.0327(8) Uani 1 1 d .
H20A H 0.2202 0.7571 0.5742 0.039 Uiso 1 1 calc R
H20B H 0.2063 0.9244 0.5288 0.039 Uiso 1 1 calc R
C21 C 0.4599(4) 0.9290(4) 0.5338(2) 0.0336(8) Uani 1 1 d .
H21A H 0.5125 0.8398 0.5243 0.040 Uiso 1 1 calc R
H21B H 0.4947 0.9837 0.5999 0.040 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'
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
C1 N1 C8 122.2(3) . .
C7 N2 C20 125.0(3) . .
C7 N2 H2 116(2) . .
C20 N2 H2 118(2) . .
N1 C1 C2 123.6(3) . .
N1 C1 C7 113.3(3) . .
C2 C1 C7 123.1(3) . .
C3 C2 C1 132.4(3) . .
C3 C2 H2A 113.8 . .
C1 C2 H2A 113.8 . .
C2 C3 C4 130.1(3) . .
C2 C3 H3A 114.9 . .
C4 C3 H3A 114.9 . .
C5 C4 C3 125.7(3) . .
C5 C4 H4A 117.1 . .
C3 C4 H4A 117.1 . .
C4 C5 C6 130.4(3) . .
C4 C5 H5A 114.8 . .
C6 C5 H5A 114.8 . .
C7 C6 C5 131.4(3) . .
C7 C6 H6A 114.3 . .
C5 C6 H6A 114.3 . .
N2 C7 C6 121.4(3) . .
N2 C7 C1 112.4(3) . .
C6 C7 C1 126.1(3) . .
C13 C8 C9 120.7(3) . .
C13 C8 N1 119.3(3) . .
C9 C8 N1 119.7(3) . .
C10 C9 C8 118.8(3) . .
C10 C9 C14 121.6(3) . .
C8 C9 C14 119.6(3) . .
C9 C10 C11 121.0(3) . .
C9 C10 H10A 119.5 . .
C11 C10 H10A 119.5 . .
C12 C11 C10 119.9(3) . .
C12 C11 H11A 120.0 . .
C10 C11 H11A 120.0 . .
C11 C12 C13 121.3(3) . .
C11 C12 H12A 119.4 . .
C13 C12 H12A 119.4 . .
C12 C13 C8 118.3(3) . .
C12 C13 C17 119.5(3) . .
C8 C13 C17 122.1(3) . .
C16 C14 C15 110.0(3) . .
C16 C14 C9 110.6(3) . .
C15 C14 C9 113.0(3) . .
C16 C14 H14A 107.7 . .
C15 C14 H14A 107.7 . .
C9 C14 H14A 107.7 . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C14 C16 H16A 109.5 . .
C14 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C14 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C18 C17 C13 111.5(3) . .
C18 C17 C19 109.9(3) . .
C13 C17 C19 111.9(3) . .
C18 C17 H17A 107.8 . .
C13 C17 H17A 107.8 . .
C19 C17 H17A 107.8 . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C17 C19 H19A 109.5 . .
C17 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C17 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
N2 C20 C21 111.7(3) . .
N2 C20 H20A 109.3 . .
C21 C20 H20A 109.3 . .
N2 C20 H20B 109.3 . .
C21 C20 H20B 109.3 . .
H20A C20 H20B 107.9 . .
C20 C21 C21 115.3(3) . 2_676
C20 C21 H21A 108.4 . .
C21 C21 H21A 108.4 2_676 .
C20 C21 H21B 108.4 . .
C21 C21 H21B 108.4 2_676 .
H21A C21 H21B 107.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C1 1.305(4) .
N1 C8 1.422(4) .
N2 C7 1.347(4) .
N2 C20 1.458(4) .
N2 H2 0.93(4) .
C1 C2 1.432(4) .
C1 C7 1.492(4) .
C2 C3 1.360(5) .
C2 H2A 0.9500 .
C3 C4 1.411(5) .
C3 H3A 0.9500 .
C4 C5 1.360(5) .
C4 H4A 0.9500 .
C5 C6 1.403(5) .
C5 H5A 0.9500 .
C6 C7 1.382(4) .
C6 H6A 0.9500 .
C8 C13 1.407(4) .
C8 C9 1.412(4) .
C9 C10 1.387(4) .
C9 C14 1.528(4) .
C10 C11 1.392(5) .
C10 H10A 0.9500 .
C11 C12 1.378(5) .
C11 H11A 0.9500 .
C12 C13 1.400(4) .
C12 H12A 0.9500 .
C13 C17 1.515(4) .
C14 C16 1.518(5) .
C14 C15 1.525(5) .
C14 H14A 1.0000 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 C18 1.510(5) .
C17 C19 1.516(5) .
C17 H17A 1.0000 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 C21 1.504(5) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C21 C21 1.524(7) 2_676
C21 H21A 0.9900 .
C21 H21B 0.9900 .
