#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:28:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179142 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/03/4310353.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_4310353
loop_
_publ_author_name
'Yanhui Shi'
'Changsheng Cao'
'Aaron L. Odom'
_publ_section_title
;
 Synthesis and Group 4 Complexes of Tris(pyrrolyl-α-methyl)amine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              275
_journal_page_last               281
_journal_paper_doi               10.1021/ic035049v
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C20 H29 Cl3 N6 Zr'
_chemical_formula_weight         551.06
_chemical_name_common            ZrCl(NHMe2)2(tpa)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.116(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.468(3)
_cell_length_b                   15.019(3)
_cell_length_c                   13.703(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2452.3(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10930
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1128
_refine_diff_density_max         1.246
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.0006(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0475P)²+4.8197P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                2986
_reflns_number_total             3522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035049vsi20030908_104650_4.cif
_cod_data_source_block           shizrtp
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2452.5(9)
_cod_database_code               4310353
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr Zr 0.29727(3) 0.34936(2) 0.53508(3) 0.01803(15) Uani 1 1 d . . .
Cl Cl 0.49060(8) 0.36008(6) 0.50767(8) 0.0258(2) Uani 1 1 d . . .
Cl1S Cl 0.78246(18) 0.18841(11) 0.48262(15) 0.0877(5) Uani 1 1 d . . .
Cl2S Cl 0.77741(15) 0.16334(15) 0.69056(16) 0.1029(7) Uani 1 1 d . . .
N1 N 0.3078(3) 0.2107(2) 0.4946(2) 0.0240(8) Uani 1 1 d . . .
N2 N 0.1824(3) 0.3758(2) 0.6261(2) 0.0231(7) Uani 1 1 d . . .
N3 N 0.2394(3) 0.4204(2) 0.3898(2) 0.0229(7) Uani 1 1 d . . .
N4 N 0.1150(3) 0.2970(2) 0.4448(2) 0.0214(7) Uani 1 1 d . . .
N5 N 0.3616(3) 0.4974(2) 0.5983(2) 0.0240(7) Uani 1 1 d . . .
N6 N 0.4039(3) 0.2956(2) 0.7051(2) 0.0259(8) Uani 1 1 d . . .
C1S C 0.7743(5) 0.2405(4) 0.5945(4) 0.0668(17) Uani 1 1 d . . .
H1SA H 0.8367 0.2815 0.6183 0.080 Uiso 1 1 calc R . .
H1SB H 0.7054 0.2747 0.5798 0.080 Uiso 1 1 calc R . .
C11 C 0.3954(4) 0.1514(3) 0.5000(3) 0.0305(10) Uani 1 1 d . . .
H11A H 0.4685 0.1679 0.5044 0.037 Uiso 1 1 calc R . .
C12 C 0.3586(4) 0.0663(3) 0.4981(3) 0.0342(10) Uani 1 1 d . . .
H12A H 0.4014 0.0150 0.5012 0.041 Uiso 1 1 calc R . .
C13 C 0.2427(4) 0.0700(3) 0.4905(3) 0.0305(10) Uani 1 1 d . . .
H13A H 0.1952 0.0217 0.4878 0.037 Uiso 1 1 calc R . .
C14 C 0.2142(3) 0.1575(2) 0.4878(3) 0.0249(9) Uani 1 1 d . . .
C15 C 0.1063(3) 0.2040(2) 0.4797(3) 0.0263(9) Uani 1 1 d . . .
H15A H 0.0920 0.2045 0.5455 0.032 Uiso 1 1 calc R . .
H15B H 0.0448 0.1734 0.4312 0.032 Uiso 1 1 calc R . .
C21 C 0.1940(3) 0.4063(3) 0.7249(3) 0.0248(9) Uani 1 1 d . . .
H21A H 0.2618 0.4099 0.7765 0.030 Uiso 1 1 calc R . .
C22 C 0.0934(3) 0.4300(3) 0.7355(3) 0.0266(9) Uani 1 1 d . . .
H22A H 0.0804 0.4528 0.7941 0.032 Uiso 1 1 calc R . .
C23 C 0.0117(3) 0.4136(3) 0.6413(3) 0.0274(9) Uani 1 1 d . . .
H23A H -0.0652 0.4231 0.6262 0.033 Uiso 1 1 calc R . .
C24 C 0.0673(3) 0.3812(2) 0.5766(3) 0.0222(9) Uani 1 1 d . . .
C25 C 0.0287(3) 0.3555(3) 0.4669(3) 0.0238(9) Uani 1 1 d . . .
H25A H 0.0178 0.4083 0.4244 0.029 Uiso 1 1 calc R . .
H25B H -0.0423 0.3241 0.4522 0.029 Uiso 1 1 calc R . .
C31 C 0.2746(3) 0.4949(3) 0.3471(3) 0.0271(9) Uani 1 1 d . . .
H31A H 0.3337 0.5319 0.3810 0.032 Uiso 1 1 calc R . .
C32 C 0.2109(4) 0.5060(3) 0.2490(3) 0.0308(10) Uani 1 1 d . . .
H32A H 0.2185 0.5510 0.2049 0.037 Uiso 1 1 calc R . .
C33 C 0.1309(3) 0.4370(3) 0.2263(3) 0.0289(10) Uani 1 1 d . . .
H33A H 0.0755 0.4280 0.1647 0.035 Uiso 1 1 calc R . .
C34 C 0.1502(3) 0.3858(3) 0.3119(3) 0.0233(9) Uani 1 1 d . . .
C35 C 0.1024(3) 0.2999(3) 0.3336(3) 0.0251(9) Uani 1 1 d . . .
H35A H 0.0238 0.2958 0.2948 0.030 Uiso 1 1 calc R . .
H35B H 0.1420 0.2504 0.3145 0.030 Uiso 1 1 calc R . .
C51 C 0.2697(4) 0.5630(3) 0.5852(3) 0.0316(10) Uani 1 1 d . . .
H51A H 0.3007 0.6196 0.6118 0.047 Uiso 1 1 calc R . .
H51B H 0.2190 0.5430 0.6215 0.047 Uiso 1 1 calc R . .
H51C H 0.2300 0.5689 0.5140 0.047 Uiso 1 1 calc R . .
C52 C 0.4431(4) 0.5095(3) 0.7012(3) 0.0332(10) Uani 1 1 d . . .
H52A H 0.4587 0.5717 0.7136 0.050 Uiso 1 1 calc R . .
H52B H 0.5113 0.4785 0.7044 0.050 Uiso 1 1 calc R . .
H52C H 0.4118 0.4860 0.7520 0.050 Uiso 1 1 calc R . .
C61 C 0.3462(4) 0.2145(3) 0.7290(3) 0.0315(10) Uani 1 1 d . . .
H61A H 0.3869 0.1925 0.7954 0.047 Uiso 1 1 calc R . .
H61B H 0.3438 0.1694 0.6788 0.047 Uiso 1 1 calc R . .
H61C H 0.2712 0.2296 0.7282 0.047 Uiso 1 1 calc R . .
C62 C 0.5256(3) 0.2760(3) 0.7331(3) 0.0360(11) Uani 1 1 d . . .
H62A H 0.5510 0.2558 0.8025 0.054 Uiso 1 1 calc R . .
H62B H 0.5657 0.3290 0.7259 0.054 Uiso 1 1 calc R . .
H62C H 0.5390 0.2305 0.6888 0.054 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'
Zr Zr -2.9673 0.5597 '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'
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
_geom_angle_publ_flag
N1 Zr N3 105.34(12) . . ?
N1 Zr N2 114.70(12) . . ?
N3 Zr N2 109.47(12) . . ?
N1 Zr N4 70.72(11) . . ?
N3 Zr N4 71.27(11) . . ?
N2 Zr N4 70.86(11) . . ?
N1 Zr N5 158.34(11) . . ?
N3 Zr N5 82.19(11) . . ?
N2 Zr N5 80.45(11) . . ?
N4 Zr N5 130.63(10) . . ?
N1 Zr N6 82.54(12) . . ?
N3 Zr N6 165.17(11) . . ?
N2 Zr N6 77.39(11) . . ?
N4 Zr N6 123.53(11) . . ?
N5 Zr N6 86.16(11) . . ?
N1 Zr Cl 83.81(9) . . ?
N3 Zr Cl 84.73(8) . . ?
N2 Zr Cl 151.04(9) . . ?
N4 Zr Cl 138.04(8) . . ?
N5 Zr Cl 76.60(8) . . ?
N6 Zr Cl 83.65(8) . . ?
C11 N1 C14 105.4(3) . . ?
C11 N1 Zr 134.8(3) . . ?
C14 N1 Zr 117.0(2) . . ?
C21 N2 C24 104.5(3) . . ?
C21 N2 Zr 135.4(3) . . ?
C24 N2 Zr 118.9(2) . . ?
C31 N3 C34 104.8(3) . . ?
C31 N3 Zr 135.6(3) . . ?
C34 N3 Zr 119.4(2) . . ?
C35 N4 C25 109.1(3) . . ?
C35 N4 C15 111.1(3) . . ?
C25 N4 C15 111.2(3) . . ?
C35 N4 Zr 108.7(2) . . ?
C25 N4 Zr 109.7(2) . . ?
C15 N4 Zr 107.0(2) . . ?
C51 N5 C52 108.8(3) . . ?
C51 N5 Zr 113.7(2) . . ?
C52 N5 Zr 120.7(2) . . ?
C62 N6 C61 107.6(3) . . ?
C62 N6 Zr 122.6(2) . . ?
C61 N6 Zr 108.3(2) . . ?
Cl2S C1S Cl1S 111.7(4) . . ?
C12 C11 N1 110.3(4) . . ?
C11 C12 C13 107.2(4) . . ?
C14 C13 C12 107.0(4) . . ?
C13 C14 N1 110.2(3) . . ?
C13 C14 C15 132.7(4) . . ?
N1 C14 C15 117.1(3) . . ?
C14 C15 N4 108.3(3) . . ?
C22 C21 N2 110.8(3) . . ?
C21 C22 C23 107.4(4) . . ?
C24 C23 C22 106.7(4) . . ?
C23 C24 N2 110.5(3) . . ?
C23 C24 C25 132.3(4) . . ?
N2 C24 C25 117.2(3) . . ?
C24 C25 N4 108.7(3) . . ?
C32 C31 N3 110.5(4) . . ?
C31 C32 C33 107.4(4) . . ?
C34 C33 C32 106.9(4) . . ?
C33 C34 N3 110.4(3) . . ?
C33 C34 C35 132.9(4) . . ?
N3 C34 C35 116.5(3) . . ?
N4 C35 C34 107.6(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr N1 2.169(3) . ?
Zr N3 2.186(3) . ?
Zr N2 2.195(3) . ?
Zr N4 2.378(3) . ?
Zr N5 2.435(3) . ?
Zr N6 2.454(3) . ?
Zr Cl 2.5515(11) . ?
Cl1S C1S 1.751(6) . ?
Cl2S C1S 1.746(6) . ?
N1 C11 1.394(5) . ?
N1 C14 1.394(5) . ?
N2 C21 1.395(5) . ?
N2 C24 1.397(5) . ?
N3 C31 1.393(5) . ?
N3 C34 1.395(5) . ?
N4 C35 1.486(5) . ?
N4 C25 1.488(5) . ?
N4 C15 1.490(5) . ?
N5 C51 1.481(5) . ?
N5 C52 1.486(5) . ?
N6 C62 1.482(5) . ?
N6 C61 1.498(5) . ?
C11 C12 1.357(6) . ?
C12 C13 1.420(6) . ?
C13 C14 1.360(5) . ?
C14 C15 1.490(5) . ?
C21 C22 1.352(6) . ?
C22 C23 1.410(6) . ?
C23 C24 1.366(5) . ?
C24 C25 1.488(5) . ?
C31 C32 1.355(6) . ?
C32 C33 1.408(6) . ?
C33 C34 1.364(6) . ?
C34 C35 1.489(6) . ?
