#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/10/7111065.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_7111065
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         'C12 H26 Cl3 N3 Zr '
_chemical_formula_sum            'C12 H26 Cl3 N3 Zr'
_chemical_formula_weight         409.94
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             'Tue Jul  4 10:40:25 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.517(1)
_cell_length_b                   10.144(1)
_cell_length_c                   22.790(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    150
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     1737.8(4)
_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      150
_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  0.0673
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7804
_diffrn_reflns_theta_max         25.59
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.085
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       needle
_exptl_crystal_F_000             840.00
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.52
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   0.760
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         1735
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_obs          0.0311
_refine_ls_shift/esd_max         0.0310
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0397
_refine_ls_wR_factor_obs         0.0316
_reflns_number_observed          1735
_reflns_number_total             2947
_reflns_observed_criterion       'I>3.00 sigma'
_cod_data_source_file            b005675hsup1.cif
_cod_data_source_block           tacnzrcl3
_cod_original_cell_volume        1738.0(3)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C12 H26 Cl3 N3 Zr '
_cod_database_code               7111065
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'1/2-x,   -y,1/2+z'
'1/2+x,1/2-y,   -z'
'   -x,1/2+y,1/2-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) 1.01657(8) 0.06806(6) 0.64383(3) 0.025 Uij
Cl(1) 0.8711(2) 0.1709(2) 0.55757(8) 0.026 Uij
Cl(2) 0.7822(2) 0.1351(2) 0.71219(8) 0.024 Uij
Cl(3) 0.8963(2) -0.1509(2) 0.62634(8) 0.025 Uij
N(1) 1.1929(6) 0.0552(5) 0.7094(2) 0.016 Uij
N(2) 1.2897(7) -0.0226(5) 0.6031(3) 0.020 Uij
N(3) 1.2086(6) 0.2672(5) 0.6379(3) 0.021 Uij
C(1) 1.2270(9) 0.1821(7) 0.7400(3) 0.021 Uij
C(2) 1.3050(9) 0.2798(7) 0.6957(3) 0.018 Uij
C(3) 1.3329(9) 0.2240(7) 0.5903(3) 0.021 Uij
C(4) 1.4200(8) 0.0897(7) 0.5981(3) 0.024 Uij
C(5) 1.3457(8) -0.1111(6) 0.6528(4) 0.021 Uij
C(6) 1.3391(9) -0.0372(7) 0.7107(3) 0.023 Uij
C(7) 1.1302(9) 0.3990(6) 0.6190(3) 0.025 Uij
C(8) 0.9780(9) 0.4392(7) 0.6591(3) 0.031 Uij
C(9) 1.265(1) 0.5099(7) 0.6125(4) 0.040 Uij
C(10) 1.2857(9) -0.1031(6) 0.5472(3) 0.021 Uij
C(11) 1.226(1) -0.0230(7) 0.4951(3) 0.028 Uij
C(12) 1.4571(10) -0.1737(7) 0.5321(4) 0.039 Uij
H(1) 1.119 0.216 0.755 0.025 Uij
H(2) 1.309 0.169 0.771 0.025 Uij
H(3) 1.292 0.367 0.710 0.022 Uij
H(4) 1.428 0.261 0.690 0.022 Uij
H(5) 1.268 0.222 0.555 0.025 Uij
H(6) 1.425 0.288 0.587 0.025 Uij
H(7) 1.495 0.074 0.565 0.029 Uij
H(8) 1.490 0.092 0.633 0.029 Uij
H(9) 1.267 -0.185 0.655 0.025 Uij
H(10) 1.464 -0.141 0.646 0.025 Uij
H(11) 1.322 -0.098 0.742 0.028 Uij
H(12) 1.448 0.009 0.716 0.028 Uij
H(13) 1.080 0.386 0.581 0.029 Uij
H(14) 0.886 0.376 0.657 0.037 Uij
H(15) 0.934 0.523 0.647 0.037 Uij
H(16) 1.020 0.445 0.698 0.037 Uij
H(17) 1.215 0.578 0.589 0.048 Uij
H(18) 1.294 0.543 0.650 0.048 Uij
H(19) 1.369 0.477 0.594 0.048 Uij
H(20) 1.199 -0.170 0.553 0.026 Uij
H(21) 1.177 -0.080 0.466 0.034 Uij
H(22) 1.137 0.038 0.507 0.034 Uij
H(23) 1.324 0.023 0.479 0.034 Uij
H(24) 1.548 -0.111 0.526 0.046 Uij
H(25) 1.490 -0.230 0.564 0.046 Uij
H(26) 1.440 -0.225 0.498 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 48 0.003 0.002 'International Tables'
H 0 104 0.000 0.000 'International Tables'
N 0 12 0.006 0.003 'International Tables'
Zr 0 4 -2.967 0.560 'International Tables'
Cl 0 12 0.148 0.159 '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
Cl(1) Zr(1) Cl(2) 94.02(7) yes
Cl(1) Zr(1) Cl(3) 95.19(6) yes
Cl(1) Zr(1) N(1) 155.7(2) yes
Cl(1) Zr(1) N(2) 103.2(1) yes
Cl(1) Zr(1) N(3) 82.6(1) yes
Cl(2) Zr(1) Cl(3) 95.20(6) yes
Cl(2) Zr(1) N(1) 91.1(2) yes
Cl(2) Zr(1) N(2) 162.7(1) yes
Cl(2) Zr(1) N(3) 103.1(1) yes
Cl(3) Zr(1) N(1) 108.0(2) yes
Cl(3) Zr(1) N(2) 84.6(1) yes
Cl(3) Zr(1) N(3) 161.7(1) yes
N(1) Zr(1) N(2) 72.7(2) yes
N(1) Zr(1) N(3) 73.1(2) yes
N(2) Zr(1) N(3) 78.3(2) yes
Zr(1) N(1) C(1) 114.0(4) yes
Zr(1) N(1) C(6) 124.1(5) yes
C(1) N(1) C(6) 114.9(5) yes
Zr(1) N(2) C(4) 106.9(4) yes
Zr(1) N(2) C(5) 100.0(4) yes
Zr(1) N(2) C(10) 120.6(4) yes
C(4) N(2) C(5) 109.0(5) yes
C(4) N(2) C(10) 111.0(5) yes
C(5) N(2) C(10) 108.5(5) yes
Zr(1) N(3) C(2) 107.5(4) yes
Zr(1) N(3) C(3) 99.4(4) yes
Zr(1) N(3) C(7) 120.3(4) yes
C(2) N(3) C(3) 110.9(5) yes
C(2) N(3) C(7) 111.0(5) yes
C(3) N(3) C(7) 107.1(5) yes
N(1) C(1) C(2) 108.5(6) yes
N(3) C(2) C(1) 109.7(5) yes
N(3) C(3) C(4) 116.4(6) yes
N(2) C(4) C(3) 113.9(5) yes
N(2) C(5) C(6) 110.5(5) yes
N(1) C(6) C(5) 109.1(6) yes
N(3) C(7) C(8) 110.9(5) yes
N(3) C(7) C(9) 114.8(6) yes
C(8) C(7) C(9) 111.2(6) yes
N(2) C(10) C(11) 112.2(5) yes
N(2) C(10) C(12) 115.4(6) yes
C(11) C(10) C(12) 109.4(6) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Zr(1) Cl(1) 2.480(2) yes
Zr(1) Cl(2) 2.449(2) yes
Zr(1) Cl(3) 2.431(2) yes
Zr(1) N(1) 2.003(5) yes
Zr(1) N(2) 2.434(5) yes
Zr(1) N(3) 2.487(5) yes
N(1) C(1) 1.486(9) yes
N(1) C(6) 1.444(8) yes
N(2) C(4) 1.506(7) yes
N(2) C(5) 1.505(9) yes
N(2) C(10) 1.513(9) yes
N(3) C(2) 1.508(9) yes
N(3) C(3) 1.498(9) yes
N(3) C(7) 1.523(7) yes
C(1) C(2) 1.532(10) yes
C(3) C(4) 1.522(9) yes
C(5) C(6) 1.52(1) yes
C(7) C(8) 1.520(9) yes
C(7) C(9) 1.521(9) yes
C(10) C(11) 1.51(1) yes
C(10) C(12) 1.514(9) yes
