#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:32:37 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179795 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/91/7009181.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_7009181
loop_
_publ_author_name
'Dawson, David M.'
'Walker, Dennis A.'
'Thornton-Pett, Mark'
'Bochmann, Manfred'
_publ_section_title
;
 Synthesis and reactivity of sterically hindered iminopyrrolato
 complexes of zirconium, iron, cobalt and nickel
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              459
_journal_paper_doi               10.1039/a909125d
_journal_year                    2000
_chemical_formula_sum            'C38 H54 N6 Zr'
_chemical_formula_weight         686.09
_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                 97.8130(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7035(2)
_cell_length_b                   11.32660(10)
_cell_length_c                   22.2836(3)
_cell_measurement_temperature    150(2)
_cell_volume                     3676.68(8)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method
;
   Detector set at 30mm from sample with different 2theta offsets 
   1 degree phi exposures for chi=0 degree settings
   1 degree omega exposures for chi=90 degree settings
;
_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  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13383
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    0.333
_exptl_absorpt_correction_T_max  0.8539
_exptl_absorpt_correction_T_min  0.8228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Using multiple and symmetry-related data measurements via the program SORTAV
 See R.H. Blessing, Acta Cryst (1995), A51, 33-38 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.61
_exptl_crystal_size_min          0.49
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0355
_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)+(0.0480P)²+1.5040P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                6675
_reflns_number_total             7069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a909125d.txt
_cod_data_source_block           MB48
_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_sg_symbol_H-M      P21/c
_cod_database_code               7009181
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
Zr1 Zr 0.321787(9) 0.343799(13) 0.159828(6) 0.02146(8) Uani 1 1 d . . .
N1 N 0.33875(9) 0.47488(12) 0.08599(6) 0.0261(3) Uani 1 1 d . . .
C2 C 0.41060(12) 0.51598(16) 0.06010(8) 0.0312(4) Uani 1 1 d . . .
H2 H 0.4731 0.4970 0.0733 0.037 Uiso 1 1 calc R . .
C3 C 0.38038(13) 0.59015(17) 0.01138(8) 0.0354(4) Uani 1 1 d . . .
H3 H 0.4177 0.6298 -0.0138 0.042 Uiso 1 1 calc R . .
C4 C 0.28520(13) 0.59493(15) 0.00687(8) 0.0330(4) Uani 1 1 d . . .
H4 H 0.2447 0.6380 -0.0220 0.040 Uiso 1 1 calc R . .
C5 C 0.26109(12) 0.52346(14) 0.05339(8) 0.0275(3) Uani 1 1 d . . .
C6 C 0.17604(11) 0.48838(15) 0.06974(7) 0.0274(3) Uani 1 1 d . . .
H6 H 0.1209 0.5203 0.0488 0.033 Uiso 1 1 calc R . .
N7 N 0.17185(9) 0.41254(12) 0.11335(6) 0.0257(3) Uani 1 1 d . . .
C71 C 0.07893(11) 0.38717(16) 0.12488(8) 0.0283(3) Uani 1 1 d . . .
C72 C 0.04276(12) 0.44774(17) 0.17138(8) 0.0329(4) Uani 1 1 d . . .
C73 C -0.04835(13) 0.4267(2) 0.17891(10) 0.0420(5) Uani 1 1 d . . .
H73 H -0.0741 0.4670 0.2100 0.050 Uiso 1 1 calc R . .
C74 C -0.10208(14) 0.34799(19) 0.14191(12) 0.0468(5) Uani 1 1 d . . .
H74 H -0.1643 0.3354 0.1473 0.056 Uiso 1 1 calc R . .
C75 C -0.06491(13) 0.28797(19) 0.09723(10) 0.0432(5) Uani 1 1 d . . .
H75 H -0.1020 0.2336 0.0723 0.052 Uiso 1 1 calc R . .
C76 C 0.02580(12) 0.30539(17) 0.08783(9) 0.0328(4) Uani 1 1 d . . .
C77 C 0.09904(13) 0.5372(2) 0.21137(9) 0.0402(4) Uani 1 1 d . . .
H77 H 0.1654 0.5202 0.2098 0.048 Uiso 1 1 calc R . .
C78 C 0.0792(2) 0.6630(2) 0.18766(13) 0.0594(7) Uani 1 1 d . . .
H78A H 0.0927 0.6686 0.1459 0.089 Uiso 1 1 calc R . .
H78B H 0.1178 0.7190 0.2132 0.089 Uiso 1 1 calc R . .
H78C H 0.0144 0.6818 0.1888 0.089 Uiso 1 1 calc R . .
C79 C 0.08245(16) 0.5290(3) 0.27753(10) 0.0579(6) Uani 1 1 d . . .
H79A H 0.0196 0.5542 0.2810 0.087 Uiso 1 1 calc R . .
H79B H 0.1260 0.5802 0.3025 0.087 Uiso 1 1 calc R . .
H79C H 0.0911 0.4472 0.2915 0.087 Uiso 1 1 calc R . .
C80 C 0.06374(12) 0.23169(17) 0.03989(9) 0.0364(4) Uani 1 1 d . . .
H80 H 0.1280 0.2585 0.0377 0.044 Uiso 1 1 calc R . .
C81 C 0.00844(15) 0.2478(3) -0.02274(10) 0.0547(6) Uani 1 1 d . . .
H81A H 0.0358 0.2002 -0.0524 0.082 Uiso 1 1 calc R . .
H81B H 0.0091 0.3313 -0.0343 0.082 Uiso 1 1 calc R . .
H81C H -0.0550 0.2224 -0.0217 0.082 Uiso 1 1 calc R . .
C82 C 0.06713(17) 0.1016(2) 0.05720(12) 0.0520(5) Uani 1 1 d . . .
H82A H 0.1082 0.0910 0.0953 0.078 Uiso 1 1 calc R . .
H82B H 0.0901 0.0556 0.0252 0.078 Uiso 1 1 calc R . .
H82C H 0.0053 0.0746 0.0623 0.078 Uiso 1 1 calc R . .
N8 N 0.47434(10) 0.32508(13) 0.16565(6) 0.0270(3) Uani 1 1 d . . .
C9 C 0.54711(12) 0.37905(18) 0.19846(8) 0.0325(4) Uani 1 1 d . . .
H9 H 0.5426 0.4329 0.2306 0.039 Uiso 1 1 calc R . .
C10 C 0.62919(13) 0.34531(17) 0.17887(9) 0.0349(4) Uani 1 1 d . . .
H10 H 0.6891 0.3715 0.1947 0.042 Uiso 1 1 calc R . .
C11 C 0.60635(12) 0.26536(17) 0.13148(8) 0.0320(4) Uani 1 1 d . . .
H11 H 0.6475 0.2259 0.1088 0.038 Uiso 1 1 calc R . .
C12 C 0.51088(11) 0.25510(15) 0.12409(7) 0.0261(3) Uani 1 1 d . . .
C13 C 0.44938(11) 0.18995(15) 0.08172(7) 0.0267(3) Uani 1 1 d . . .
H13 H 0.4737 0.1395 0.0538 0.032 Uiso 1 1 calc R . .
N14 N 0.36114(9) 0.19738(12) 0.08013(6) 0.0248(3) Uani 1 1 d . . .
C141 C 0.31032(11) 0.12060(15) 0.03546(7) 0.0263(3) Uani 1 1 d . . .
C142 C 0.27979(12) 0.16394(15) -0.02287(8) 0.0281(4) Uani 1 1 d . . .
C143 C 0.23723(12) 0.08468(17) -0.06589(8) 0.0339(4) Uani 1 1 d . . .
H143 H 0.2150 0.1124 -0.1054 0.041 Uiso 1 1 calc R . .
C144 C 0.22680(14) -0.03302(18) -0.05223(9) 0.0388(4) Uani 1 1 d . . .
H144 H 0.1997 -0.0859 -0.0826 0.047 Uiso 1 1 calc R . .
C145 C 0.25586(14) -0.07389(17) 0.00575(9) 0.0374(4) Uani 1 1 d . . .
H145 H 0.2475 -0.1547 0.0150 0.045 Uiso 1 1 calc R . .
C146 C 0.29723(12) 0.00175(16) 0.05087(8) 0.0311(4) Uani 1 1 d . . .
C147 C 0.29916(13) 0.28964(16) -0.04156(8) 0.0317(4) Uani 1 1 d . . .
H147 H 0.3092 0.3391 -0.0041 0.038 Uiso 1 1 calc R . .
C148 C 0.38751(14) 0.2919(2) -0.07058(9) 0.0431(5) Uani 1 1 d . . .
H14A H 0.4389 0.2647 -0.0411 0.065 Uiso 1 1 calc R . .
H14B H 0.3995 0.3726 -0.0832 0.065 Uiso 1 1 calc R . .
H14C H 0.3809 0.2397 -0.1060 0.065 Uiso 1 1 calc R . .
C149 C 0.22102(16) 0.34529(18) -0.08469(10) 0.0427(5) Uani 1 1 d . . .
H14D H 0.2121 0.3009 -0.1228 0.064 Uiso 1 1 calc R . .
H14E H 0.2365 0.4274 -0.0928 0.064 Uiso 1 1 calc R . .
H14F H 0.1644 0.3432 -0.0661 0.064 Uiso 1 1 calc R . .
C150 C 0.32976(14) -0.04678(17) 0.11363(9) 0.0389(4) Uani 1 1 d . . .
H150 H 0.3415 0.0218 0.1419 0.047 Uiso 1 1 calc R . .
C151 C 0.25799(17) -0.1259(2) 0.13741(10) 0.0499(5) Uani 1 1 d . . .
H15A H 0.1981 -0.0865 0.1313 0.075 Uiso 1 1 calc R . .
H15B H 0.2761 -0.1407 0.1807 0.075 Uiso 1 1 calc R . .
H15C H 0.2539 -0.2011 0.1154 0.075 Uiso 1 1 calc R . .
C152 C 0.41982(16) -0.1145(2) 0.11473(11) 0.0538(6) Uani 1 1 d . . .
H15D H 0.4105 -0.1817 0.0868 0.081 Uiso 1 1 calc R . .
H15E H 0.4400 -0.1433 0.1559 0.081 Uiso 1 1 calc R . .
H15F H 0.4668 -0.0620 0.1022 0.081 Uiso 1 1 calc R . .
N15 N 0.34201(10) 0.46769(13) 0.22721(6) 0.0293(3) Uani 1 1 d . . .
C16 C 0.38543(15) 0.58261(18) 0.22181(9) 0.0416(4) Uani 1 1 d . . .
H16A H 0.3411 0.6454 0.2264 0.062 Uiso 1 1 calc R . .
H16B H 0.4060 0.5891 0.1819 0.062 Uiso 1 1 calc R . .
H16C H 0.4383 0.5904 0.2534 0.062 Uiso 1 1 calc R . .
C17 C 0.32078(13) 0.45443(18) 0.28908(8) 0.0372(4) Uani 1 1 d . . .
H17A H 0.3780 0.4495 0.3172 0.056 Uiso 1 1 calc R . .
H17B H 0.2849 0.3822 0.2920 0.056 Uiso 1 1 calc R . .
H17C H 0.2851 0.5227 0.2996 0.056 Uiso 1 1 calc R . .
N18 N 0.25726(10) 0.21987(13) 0.20587(6) 0.0283(3) Uani 1 1 d . . .
C19 C 0.17110(14) 0.17082(19) 0.21884(10) 0.0398(5) Uani 1 1 d . . .
H19A H 0.1700 0.0857 0.2108 0.060 Uiso 1 1 calc R . .
H19B H 0.1202 0.2089 0.1930 0.060 Uiso 1 1 calc R . .
H19C H 0.1648 0.1846 0.2615 0.060 Uiso 1 1 calc R . .
C20 C 0.33346(14) 0.16514(17) 0.24514(9) 0.0361(4) Uani 1 1 d . . .
H20A H 0.3256 0.1780 0.2876 0.054 Uiso 1 1 calc R . .
H20B H 0.3915 0.2006 0.2372 0.054 Uiso 1 1 calc R . .
H20C H 0.3344 0.0802 0.2369 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'
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
N18 Zr1 N15 97.67(6) . . ?
N18 Zr1 N8 115.79(6) . . ?
N15 Zr1 N8 88.74(5) . . ?
N18 Zr1 N1 157.25(5) . . ?
N15 Zr1 N1 93.69(6) . . ?
N8 Zr1 N1 83.99(5) . . ?
N18 Zr1 N7 88.73(5) . . ?
N15 Zr1 N7 97.23(5) . . ?
N8 Zr1 N7 153.85(5) . . ?
N1 Zr1 N7 70.27(5) . . ?
N18 Zr1 N14 93.87(5) . . ?
N15 Zr1 N14 158.65(5) . . ?
N8 Zr1 N14 70.05(5) . . ?
N1 Zr1 N14 82.08(5) . . ?
N7 Zr1 N14 100.94(4) . . ?
C2 N1 C5 106.03(14) . . ?
C2 N1 Zr1 135.04(12) . . ?
C5 N1 Zr1 118.71(11) . . ?
N1 C2 C3 110.72(16) . . ?
C4 C3 C2 106.88(15) . . ?
C3 C4 C5 106.14(16) . . ?
N1 C5 C4 110.22(15) . . ?
N1 C5 C6 116.85(14) . . ?
C4 C5 C6 132.80(16) . . ?
N7 C6 C5 120.83(15) . . ?
C6 N7 C71 113.74(13) . . ?
C6 N7 Zr1 113.33(10) . . ?
C71 N7 Zr1 132.92(10) . . ?
C76 C71 C72 121.25(16) . . ?
C76 C71 N7 119.18(15) . . ?
C72 C71 N7 119.54(15) . . ?
C73 C72 C71 118.14(17) . . ?
C73 C72 C77 119.99(17) . . ?
C71 C72 C77 121.83(16) . . ?
C74 C73 C72 121.19(18) . . ?
C75 C74 C73 119.79(18) . . ?
C74 C75 C76 121.40(19) . . ?
C75 C76 C71 118.20(17) . . ?
C75 C76 C80 118.59(17) . . ?
C71 C76 C80 123.16(15) . . ?
C72 C77 C79 112.31(19) . . ?
C72 C77 C78 110.78(17) . . ?
C79 C77 C78 109.9(2) . . ?
C76 C80 C82 110.85(18) . . ?
C76 C80 C81 112.05(16) . . ?
C82 C80 C81 110.02(18) . . ?
C9 N8 C12 105.65(14) . . ?
C9 N8 Zr1 134.34(12) . . ?
C12 N8 Zr1 119.55(11) . . ?
N8 C9 C10 111.18(16) . . ?
C9 C10 C11 106.60(16) . . ?
C12 C11 C10 106.11(16) . . ?
N8 C12 C11 110.47(15) . . ?
N8 C12 C13 118.21(14) . . ?
C11 C12 C13 131.30(16) . . ?
N14 C13 C12 121.90(15) . . ?
C13 N14 C141 113.60(14) . . ?
C13 N14 Zr1 110.11(11) . . ?
C141 N14 Zr1 136.27(10) . . ?
C142 C141 C146 121.49(16) . . ?
C142 C141 N14 119.71(15) . . ?
C146 C141 N14 118.71(15) . . ?
C143 C142 C141 117.85(16) . . ?
C143 C142 C147 119.76(16) . . ?
C141 C142 C147 122.16(15) . . ?
C144 C143 C142 121.45(17) . . ?
C143 C144 C145 119.95(17) . . ?
C144 C145 C146 121.07(18) . . ?
C145 C146 C141 118.13(17) . . ?
C145 C146 C150 119.55(17) . . ?
C141 C146 C150 122.28(16) . . ?
C142 C147 C148 109.45(16) . . ?
C142 C147 C149 113.89(15) . . ?
C148 C147 C149 109.66(16) . . ?
C146 C150 C152 111.13(17) . . ?
C146 C150 C151 112.62(17) . . ?
C152 C150 C151 109.68(18) . . ?
C16 N15 C17 108.71(15) . . ?
C16 N15 Zr1 124.85(12) . . ?
C17 N15 Zr1 126.36(12) . . ?
C19 N18 C20 109.75(14) . . ?
C19 N18 Zr1 147.26(12) . . ?
C20 N18 Zr1 102.77(11) . . ?
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
Zr1 N18 2.0465(14) . ?
Zr1 N15 2.0472(15) . ?
Zr1 N8 2.2392(14) . ?
Zr1 N1 2.2551(14) . ?
Zr1 N7 2.4327(13) . ?
Zr1 N14 2.5532(14) . ?
N1 C2 1.353(2) . ?
N1 C5 1.382(2) . ?
C2 C3 1.397(3) . ?
C3 C4 1.390(3) . ?
C4 C5 1.398(2) . ?
C5 C6 1.407(2) . ?
C6 N7 1.305(2) . ?
N7 C71 1.453(2) . ?
C71 C76 1.405(3) . ?
C71 C72 1.406(2) . ?
C72 C73 1.393(3) . ?
C72 C77 1.518(3) . ?
C73 C74 1.386(3) . ?
C74 C75 1.378(3) . ?
C75 C76 1.392(3) . ?
C76 C80 1.520(3) . ?
C77 C79 1.529(3) . ?
C77 C78 1.534(3) . ?
C80 C82 1.522(3) . ?
C80 C81 1.528(3) . ?
N8 C9 1.357(2) . ?
N8 C12 1.382(2) . ?
C9 C10 1.391(3) . ?
C10 C11 1.397(3) . ?
C11 C12 1.396(2) . ?
C12 C13 1.422(2) . ?
C13 N14 1.296(2) . ?
N14 C141 1.450(2) . ?
C141 C142 1.405(2) . ?
C141 C146 1.409(2) . ?
C142 C143 1.398(2) . ?
C142 C147 1.521(2) . ?
C143 C144 1.381(3) . ?
C144 C145 1.384(3) . ?
C145 C146 1.396(3) . ?
C146 C150 1.518(3) . ?
C147 C148 1.528(3) . ?
C147 C149 1.530(3) . ?
C150 C152 1.528(3) . ?
C150 C151 1.533(3) . ?
N15 C16 1.462(2) . ?
N15 C17 1.462(2) . ?
N18 C19 1.448(2) . ?
N18 C20 1.462(2) . ?
