#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/10/7111066.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7111066
loop_
_publ_author_name
'Giesbrecht, Garth R.'
'Shafir, Alex'
'Arnold, John'
_publ_contact_author
;
 John Arnold
 Dept of Chemistry, UC Berkeley, Berkeley, CA 94720-1460
;
_publ_section_title
;
 Zirconium complexes of a tacn-derived amido ligand and ring-opening to
 form a new diamido-amino pincer
;
_journal_issue                   21
_journal_name_full               'Chemical Communications'
_journal_page_first              2135
_journal_paper_doi               10.1039/b005675h
_journal_year                    2000
_chemical_formula_moiety         'C33 H47 N3 Zr '
_chemical_formula_sum            'C33 H47 N3 Zr'
_chemical_formula_weight         576.97
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_audit_creation_date             'Tue Jul  4 11:19:35 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   39.6517(3)
_cell_length_b                   39.6517(3)
_cell_length_c                   9.74690(10)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    173
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     13271.5(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      173
_diffrn_measurement_device       'SMART CCD'
_diffrn_measurement_method       'omega scans with profile analysis'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20082
_diffrn_reflns_theta_max         25.67
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             5508.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.34
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.008
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         3539
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_obs          0.0236
_refine_ls_shift/esd_max         0.0030
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0315
_refine_ls_wR_factor_obs         0.0280
_reflns_number_observed          3539
_reflns_number_total             5097
_reflns_observed_criterion       'I>3.00 sigma'
_cod_data_source_file            b005675hsup1.cif
_cod_data_source_block           tacn_zirconium_tribenzyl
_cod_original_sg_symbol_H-M      'R -3       '
_cod_original_formula_sum        'C33 H47 N3 Zr '
_cod_database_code               7111066
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
2/3+x,1/3+y,1/3+z
1/3+x,2/3+y,2/3+z
'   -y,   +x-y,   +z'
2/3-y,1/3+x-y,1/3+z
1/3-y,2/3+x-y,2/3+z
'   -x+y,   -x,   +z'
2/3-x+y,1/3-x,1/3+z
1/3-x+y,2/3-x,2/3+z
'   -x,   -y,   -z'
2/3-x,1/3-y,1/3-z
1/3-x,2/3-y,2/3-z
'   +y,   -x+y,   -z'
2/3+y,1/3-x+y,1/3-z
1/3+y,2/3-x+y,2/3-z
'   +x-y,   +x,   -z'
2/3+x-y,1/3+x,1/3-z
1/3+x-y,2/3+x,2/3-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
Zr(1) 0.812497(6) 0.004209(6) 1.12621(2) 0.025 Uij
N(1) 0.76096(6) -0.02636(6) 1.0172(2) 0.023 Uij
N(2) 0.82568(5) 0.01841(5) 0.8650(2) 0.018 Uij
N(3) 0.79096(5) 0.05164(5) 1.0643(2) 0.018 Uij
C(1) 0.88059(7) 0.04230(7) 1.1387(2) 0.022 Uij
C(2) 0.90141(7) 0.02298(7) 1.1967(3) 0.022 Uij
C(3) 0.92393(7) 0.01256(8) 1.1159(3) 0.028 Uij
C(4) 0.94125(7) -0.00718(8) 1.1712(3) 0.032 Uij
C(5) 0.93687(8) -0.01750(8) 1.3076(3) 0.034 Uij
C(6) 0.91514(8) -0.00706(9) 1.3898(3) 0.036 Uij
C(7) 0.89818(8) 0.01302(8) 1.3343(3) 0.031 Uij
C(8) 0.80885(7) -0.05497(7) 1.1743(3) 0.024 Uij
C(9) 0.77859(8) -0.07887(7) 1.2768(3) 0.025 Uij
C(10) 0.78784(8) -0.08068(8) 1.4137(3) 0.033 Uij
C(11) 0.7595(1) -0.10209(9) 1.5097(3) 0.046 Uij
C(12) 0.7208(1) -0.12219(9) 1.4736(4) 0.048 Uij
C(13) 0.71060(8) -0.12047(8) 1.3395(3) 0.042 Uij
C(14) 0.73896(8) -0.09902(7) 1.2416(3) 0.031 Uij
C(15) 0.80653(7) 0.01864(7) 1.3506(2) 0.021 Uij
C(16) 0.77359(7) 0.01602(7) 1.4327(2) 0.020 Uij
C(17) 0.73899(7) -0.01910(7) 1.4487(3) 0.024 Uij
C(18) 0.70819(7) -0.02170(8) 1.5239(3) 0.030 Uij
C(19) 0.71055(8) 0.01089(8) 1.5849(3) 0.032 Uij
C(20) 0.74455(8) 0.04604(7) 1.5708(3) 0.027 Uij
C(21) 0.77561(7) 0.04870(7) 1.4970(2) 0.024 Uij
C(22) 0.76342(7) -0.04335(7) 0.8872(3) 0.027 Uij
C(23) 0.78996(7) -0.01106(7) 0.7887(3) 0.024 Uij
C(24) 0.83059(7) 0.05799(7) 0.8519(2) 0.020 Uij
C(25) 0.79770(7) 0.06179(7) 0.9156(3) 0.022 Uij
C(26) 0.74842(7) 0.02526(8) 1.0930(3) 0.026 Uij
C(27) 0.73268(7) -0.01307(8) 1.0155(3) 0.028 Uij
C(28) 0.86145(7) 0.01883(7) 0.8099(2) 0.022 Uij
C(29) 0.85992(8) -0.01946(7) 0.8402(3) 0.029 Uij
C(30) 0.86947(8) 0.02849(8) 0.6584(3) 0.032 Uij
C(31) 0.80652(8) 0.08728(7) 1.1547(3) 0.026 Uij
C(32) 0.84916(8) 0.11503(7) 1.1270(3) 0.027 Uij
C(33) 0.78350(8) 0.10862(8) 1.1478(3) 0.038 Uij
H(1) 0.887 0.064 1.194 0.027 Uij
H(2) 0.890 0.051 1.048 0.027 Uij
H(3) 0.927 0.019 1.021 0.034 Uij
H(4) 0.956 -0.014 1.112 0.038 Uij
H(5) 0.949 -0.031 1.342 0.041 Uij
H(6) 0.912 -0.014 1.485 0.043 Uij
H(7) 0.884 0.020 1.393 0.037 Uij
H(8) 0.833 -0.050 1.209 0.028 Uij
H(9) 0.803 -0.069 1.092 0.028 Uij
H(10) 0.814 -0.067 1.442 0.040 Uij
H(11) 0.767 -0.103 1.602 0.055 Uij
H(12) 0.701 -0.137 1.540 0.058 Uij
H(13) 0.684 -0.134 1.314 0.050 Uij
H(14) 0.731 -0.098 1.150 0.037 Uij
H(15) 0.814 0.003 1.401 0.026 Uij
H(16) 0.826 0.045 1.359 0.026 Uij
H(17) 0.736 -0.042 1.407 0.029 Uij
H(18) 0.685 -0.046 1.534 0.036 Uij
H(19) 0.689 0.009 1.635 0.038 Uij
H(20) 0.747 0.069 1.612 0.033 Uij
H(21) 0.799 0.073 1.490 0.029 Uij
H(22) 0.774 -0.060 0.903 0.032 Uij
H(23) 0.738 -0.058 0.848 0.032 Uij
H(24) 0.797 -0.022 0.716 0.029 Uij
H(25) 0.777 0.001 0.753 0.029 Uij
H(26) 0.832 0.064 0.757 0.024 Uij
H(27) 0.854 0.076 0.896 0.024 Uij
H(28) 0.774 0.045 0.867 0.027 Uij
H(29) 0.804 0.088 0.905 0.027 Uij
H(30) 0.735 0.038 1.065 0.032 Uij
H(31) 0.745 0.020 1.189 0.032 Uij
H(32) 0.709 -0.032 1.058 0.034 Uij
H(33) 0.727 -0.009 0.923 0.034 Uij
H(34) 0.883 0.039 0.859 0.027 Uij
H(35) 0.858 -0.024 0.937 0.035 Uij
H(36) 0.838 -0.040 0.797 0.035 Uij
H(37) 0.883 -0.019 0.806 0.035 Uij
H(38) 0.895 0.033 0.636 0.038 Uij
H(39) 0.850 0.008 0.605 0.038 Uij
H(40) 0.869 0.051 0.639 0.038 Uij
H(41) 0.805 0.079 1.247 0.031 Uij
H(42) 0.863 0.101 1.128 0.032 Uij
H(43) 0.852 0.127 1.040 0.032 Uij
H(44) 0.859 0.135 1.196 0.032 Uij
H(45) 0.783 0.116 1.056 0.046 Uij
H(46) 0.795 0.131 1.205 0.046 Uij
H(47) 0.758 0.092 1.178 0.046 Uij
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 594 0.003 0.002 'International Tables'
H 0 846 0.000 0.000 'International Tables'
N 0 54 0.006 0.003 'International Tables'
Zr 0 18 -2.967 0.560 'International Tables'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N(1) Zr(1) N(2) 70.00(7) yes
N(1) Zr(1) N(3) 73.03(7) yes
N(1) Zr(1) C(1) 152.07(8) yes
N(1) Zr(1) C(8) 88.13(8) yes
N(1) Zr(1) C(15) 116.00(8) yes
N(2) Zr(1) N(3) 73.02(6) yes
N(2) Zr(1) C(1) 82.50(7) yes
N(2) Zr(1) C(8) 108.64(7) yes
N(2) Zr(1) C(15) 155.45(7) yes
N(3) Zr(1) C(1) 104.15(8) yes
N(3) Zr(1) C(8) 159.47(7) yes
N(3) Zr(1) C(15) 85.77(7) yes
C(1) Zr(1) C(8) 96.32(9) yes
C(1) Zr(1) C(15) 91.08(8) yes
C(8) Zr(1) C(15) 95.57(8) yes
Zr(1) N(1) C(22) 116.1(1) yes
Zr(1) N(1) C(27) 120.4(2) yes
C(22) N(1) C(27) 113.4(2) yes
Zr(1) N(2) C(23) 107.8(1) yes
Zr(1) N(2) C(24) 102.6(1) yes
Zr(1) N(2) C(28) 115.9(1) yes
C(23) N(2) C(24) 110.6(2) yes
C(23) N(2) C(28) 110.3(2) yes
C(24) N(2) C(28) 109.4(2) yes
Zr(1) N(3) C(25) 110.8(1) yes
Zr(1) N(3) C(26) 96.8(1) yes
Zr(1) N(3) C(31) 115.5(1) yes
C(25) N(3) C(26) 110.9(2) yes
C(25) N(3) C(31) 112.3(2) yes
C(26) N(3) C(31) 109.5(2) yes
Zr(1) C(1) C(2) 116.3(2) yes
C(1) C(2) C(3) 122.5(2) yes
C(1) C(2) C(7) 121.2(2) yes
C(3) C(2) C(7) 116.2(2) yes
C(2) C(3) C(4) 121.3(2) yes
C(3) C(4) C(5) 121.3(2) yes
C(4) C(5) C(6) 118.4(2) yes
C(5) C(6) C(7) 120.0(3) yes
C(2) C(7) C(6) 122.7(2) yes
Zr(1) C(8) C(9) 113.7(2) yes
C(8) C(9) C(10) 121.9(2) yes
C(8) C(9) C(14) 121.2(2) yes
C(10) C(9) C(14) 116.9(2) yes
C(9) C(10) C(11) 121.7(3) yes
C(10) C(11) C(12) 120.8(3) yes
C(11) C(12) C(13) 119.0(3) yes
C(12) C(13) C(14) 120.8(3) yes
C(9) C(14) C(13) 120.8(3) yes
Zr(1) C(15) C(16) 133.4(2) yes
C(15) C(16) C(17) 121.4(2) yes
C(15) C(16) C(21) 122.1(2) yes
C(17) C(16) C(21) 116.5(2) yes
C(16) C(17) C(18) 121.7(2) yes
C(17) C(18) C(19) 120.9(2) yes
C(18) C(19) C(20) 118.5(2) yes
C(19) C(20) C(21) 120.8(2) yes
C(16) C(21) C(20) 121.6(2) yes
N(1) C(22) C(23) 109.7(2) yes
N(2) C(23) C(22) 109.1(2) yes
N(2) C(24) C(25) 113.8(2) yes
N(3) C(25) C(24) 114.6(2) yes
N(3) C(26) C(27) 111.1(2) yes
N(1) C(27) C(26) 110.4(2) yes
N(2) C(28) C(29) 110.6(2) yes
N(2) C(28) C(30) 115.2(2) yes
C(29) C(28) C(30) 109.9(2) yes
N(3) C(31) C(32) 111.2(2) yes
N(3) C(31) C(33) 114.5(2) yes
C(32) C(31) C(33) 110.5(2) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Zr(1) N(1) 2.073(2) yes
Zr(1) N(2) 2.604(2) yes
Zr(1) N(3) 2.497(2) yes
Zr(1) C(1) 2.347(2) yes
Zr(1) C(8) 2.326(2) yes
Zr(1) C(15) 2.303(2) yes
N(1) C(22) 1.462(3) yes
N(1) C(27) 1.458(3) yes
N(2) C(23) 1.506(3) yes
N(2) C(24) 1.487(3) yes
N(2) C(28) 1.509(3) yes
N(3) C(25) 1.492(3) yes
N(3) C(26) 1.501(3) yes
N(3) C(31) 1.511(3) yes
C(1) C(2) 1.490(3) yes
C(2) C(3) 1.399(3) yes
C(2) C(7) 1.386(3) yes
C(3) C(4) 1.383(4) yes
C(4) C(5) 1.376(4) yes
C(5) C(6) 1.383(4) yes
C(6) C(7) 1.384(4) yes
C(8) C(9) 1.483(3) yes
C(9) C(10) 1.396(4) yes
C(9) C(14) 1.403(4) yes
C(10) C(11) 1.381(4) yes
C(11) C(12) 1.374(4) yes
C(12) C(13) 1.380(4) yes
C(13) C(14) 1.393(4) yes
C(15) C(16) 1.490(3) yes
C(16) C(17) 1.391(3) yes
C(16) C(21) 1.405(3) yes
C(17) C(18) 1.383(3) yes
C(18) C(19) 1.382(4) yes
C(19) C(20) 1.378(4) yes
C(20) C(21) 1.384(3) yes
C(22) C(23) 1.523(3) yes
C(24) C(25) 1.518(3) yes
C(26) C(27) 1.524(4) yes
C(28) C(29) 1.518(3) yes
C(28) C(30) 1.519(3) yes
C(31) C(32) 1.511(4) yes
C(31) C(33) 1.525(3) yes
