#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:26:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179328 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/25/4322528.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_4322528
loop_
_publ_author_name
'Lena Kakaliou'
Scanlon
'Baixin Qian'
'Sung W. Baek'
'Milton R. Smith'
'Douglas H. Motry'
_publ_section_title
;
 Five- and Six-Coordinate Group 4 Compounds Stabilized by β-Ketiminate
 and Diketiminate Ligands: Syntheses and Comparisons between Solid-State
 and Solution Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5964
_journal_page_last               5977
_journal_paper_doi               10.1021/ic981364j
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C28 H40 N4 O2 Zr'
_chemical_formula_weight         555.86
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 98.15(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.272(4)
_cell_length_b                   9.102(2)
_cell_length_c                   17.200(3)
_cell_measurement_temperature    173(2)
_cell_volume                     2831.7(10)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0752
_diffrn_reflns_av_sigmaI/netI    0.1271
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14661
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.418
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.987
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_restrained_S_obs      1.078
_refine_ls_R_factor_all          0.1500
_refine_ls_R_factor_obs          0.0771
_refine_ls_shift/esd_max         -0.018
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1958
_refine_ls_wR_factor_obs         0.1613
_reflns_number_observed          3714
_reflns_number_total             6399
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981364j_01.cif
_cod_data_source_block           Zr(TP)2(NMe2)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2831.5(10)
_cod_database_code               4322528
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Zr1 Zr 0.73777(3) 0.89924(6) 0.76316(3) 0.0252(2) Uani 1 d . .
O1 O 0.7109(2) 0.8796(4) 0.6437(2) 0.0312(9) Uani 1 d . .
O2 O 0.7744(2) 0.9754(5) 0.8740(2) 0.0318(9) Uani 1 d . .
N1 N 0.8356(2) 1.0252(5) 0.7130(3) 0.0295(11) Uani 1 d . .
N2 N 0.6876(2) 1.1432(5) 0.7609(3) 0.0288(11) Uani 1 d . .
N3 N 0.8031(2) 0.7117(5) 0.7752(3) 0.0303(11) Uani 1 d . .
N4 N 0.6354(2) 0.8289(6) 0.7878(3) 0.0321(11) Uani 1 d . .
C1 C 0.6831(4) 0.8673(8) 0.5058(3) 0.048(2) Uani 1 d . .
H1A H 0.6418(4) 0.8153(8) 0.5212(3) 0.072 Uiso 1 calc R .
H1B H 0.7100(4) 0.8033(8) 0.4756(3) 0.072 Uiso 1 calc R .
H1C H 0.6657(4) 0.9509(8) 0.4745(3) 0.072 Uiso 1 calc R .
C2 C 0.7329(3) 0.9176(7) 0.5775(3) 0.0326(14) Uani 1 d . .
C3 C 0.7963(3) 0.9943(7) 0.5741(3) 0.0362(15) Uani 1 d . .
H3A H 0.8079(3) 1.0151(7) 0.5244(3) 0.043 Uiso 1 calc R .
C4 C 0.8469(3) 1.0460(7) 0.6399(3) 0.0340(14) Uani 1 d . .
C5 C 0.9159(3) 1.1228(8) 0.6219(4) 0.048(2) Uani 1 d . .
H5A H 0.9453(3) 1.1524(8) 0.6700(4) 0.073 Uiso 1 calc R .
H5B H 0.9023(3) 1.2079(8) 0.5901(4) 0.073 Uiso 1 calc R .
H5C H 0.9439(3) 1.0569(8) 0.5940(4) 0.073 Uiso 1 calc R .
C6 C 0.8902(3) 1.0818(6) 0.7742(3) 0.0277(13) Uani 1 d . .
C7 C 0.8872(3) 1.2237(7) 0.7992(4) 0.040(2) Uani 1 d . .
H7A H 0.8511(3) 1.2864(7) 0.7743(4) 0.048 Uiso 1 calc R .
C8 C 0.9376(3) 1.2760(8) 0.8617(4) 0.044(2) Uani 1 d . .
H8A H 0.9349(3) 1.3734(8) 0.8775(4) 0.053 Uiso 1 calc R .
C9 C 0.9914(3) 1.1854(7) 0.9005(3) 0.0330(14) Uani 1 d . .
C10 C 0.9942(3) 1.0435(7) 0.8738(4) 0.039(2) Uani 1 d . .
H10A H 1.0313(3) 0.9815(7) 0.8975(4) 0.047 Uiso 1 calc R .
C11 C 0.9443(3) 0.9899(7) 0.8130(4) 0.0353(14) Uani 1 d . .
H11A H 0.9467(3) 0.8922(7) 0.7979(4) 0.042 Uiso 1 calc R .
C13 C 0.6447(3) 1.3788(7) 0.8106(4) 0.041(2) Uani 1 d . .
H13A H 0.6195(3) 1.3881(7) 0.7579(4) 0.062 Uiso 1 calc R .
H13B H 0.6781(3) 1.4598(7) 0.8221(4) 0.062 Uiso 1 calc R .
H13C H 0.6092(3) 1.3792(7) 0.8467(4) 0.062 Uiso 1 calc R .
C14 C 0.6878(3) 1.2354(7) 0.8185(3) 0.0324(14) Uani 1 d . .
C15 C 0.7279(3) 1.2111(7) 0.8954(3) 0.0351(14) Uani 1 d . .
H15A H 0.7262(3) 1.2855(7) 0.9321(3) 0.042 Uiso 1 calc R .
C16 C 0.7684(3) 1.0890(7) 0.9197(3) 0.0333(14) Uani 1 d . .
C17 C 0.8101(3) 1.0761(8) 1.0009(3) 0.048(2) Uani 1 d . .
H17A H 0.8350(3) 0.9830(8) 1.0065(3) 0.072 Uiso 1 calc R .
H17B H 0.7763(3) 1.0832(8) 1.0387(3) 0.072 Uiso 1 calc R .
H17C H 0.8458(3) 1.1539(8) 1.0096(3) 0.072 Uiso 1 calc R .
C18 C 0.6465(3) 1.1832(6) 0.6864(3) 0.0282(13) Uani 1 d . .
C19 C 0.6699(3) 1.2928(7) 0.6401(4) 0.040(2) Uani 1 d . .
H19A H 0.7132(3) 1.3440(7) 0.6574(4) 0.048 Uiso 1 calc R .
C20 C 0.6296(3) 1.3270(8) 0.5684(4) 0.043(2) Uani 1 d . .
H20A H 0.6461(3) 1.4025(8) 0.5389(4) 0.052 Uiso 1 calc R .
C21 C 0.5656(3) 1.2534(7) 0.5387(3) 0.0363(15) Uani 1 d . .
C22 C 0.5428(3) 1.1418(7) 0.5853(3) 0.0331(14) Uani 1 d . .
H22A H 0.4997(3) 1.0903(7) 0.5676(3) 0.040 Uiso 1 calc R .
C23 C 0.5827(3) 1.1054(7) 0.6573(3) 0.0298(12) Uani 1 d . .
H23A H 0.5669(3) 1.0285(7) 0.6864(3) 0.036 Uiso 1 calc R .
C26 C 0.8251(4) 0.6405(7) 0.8494(4) 0.042(2) Uani 1 d . .
H26A H 0.8004(4) 0.6858(7) 0.8889(4) 0.063 Uiso 1 calc R .
H26B H 0.8776(4) 0.6497(7) 0.8637(4) 0.063 Uiso 1 calc R .
H26C H 0.8120(4) 0.5384(7) 0.8451(4) 0.063 Uiso 1 calc R .
C28 C 0.5884(3) 0.7232(7) 0.7400(4) 0.043(2) Uani 1 d . .
H28A H 0.6156(3) 0.6801(7) 0.7019(4) 0.064 Uiso 1 calc R .
H28B H 0.5455(3) 0.7726(7) 0.7135(4) 0.064 Uiso 1 calc R .
H28C H 0.5733(3) 0.6476(7) 0.7732(4) 0.064 Uiso 1 calc R .
C27 C 0.5949(3) 0.8948(8) 0.8458(3) 0.0405(15) Uani 1 d . .
H27A H 0.6260(3) 0.9642(8) 0.8768(3) 0.061 Uiso 1 calc R .
H27B H 0.5799(3) 0.8194(8) 0.8793(3) 0.061 Uiso 1 calc R .
H27C H 0.5519(3) 0.9442(8) 0.8196(3) 0.061 Uiso 1 calc R .
C12 C 1.0467(3) 1.2423(8) 0.9684(4) 0.043(2) Uani 1 d . .
H12A H 1.0354(3) 1.3428(8) 0.9790(4) 0.065 Uiso 1 calc R .
H12B H 1.0957(3) 1.2362(8) 0.9547(4) 0.065 Uiso 1 calc R .
H12C H 1.0437(3) 1.1839(8) 1.0143(4) 0.065 Uiso 1 calc R .
C25 C 0.8404(4) 0.6437(8) 0.7151(4) 0.046(2) Uani 1 d . .
H25A H 0.8257(4) 0.6919(8) 0.6657(4) 0.070 Uiso 1 calc R .
H25B H 0.8272(4) 0.5416(8) 0.7105(4) 0.070 Uiso 1 calc R .
H25C H 0.8929(4) 0.6525(8) 0.7295(4) 0.070 Uiso 1 calc R .
C24 C 0.5206(4) 1.2921(9) 0.4613(3) 0.054(2) Uani 1 d . .
H24A H 0.4783(4) 1.2287(9) 0.4520(3) 0.080 Uiso 1 calc R .
H24B H 0.5503(4) 1.2800(9) 0.4200(3) 0.080 Uiso 1 calc R .
H24C H 0.5045(4) 1.3924(9) 0.4626(3) 0.080 Uiso 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'
O O 0.0106 0.0060 '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
O2 Zr1 O1 164.0(2) . . ?
O2 Zr1 N4 95.7(2) . . ?
O1 Zr1 N4 94.7(2) . . ?
O2 Zr1 N3 94.5(2) . . ?
O1 Zr1 N3 94.6(2) . . ?
N4 Zr1 N3 104.4(2) . . ?
O2 Zr1 N1 90.7(2) . . ?
O1 Zr1 N1 76.4(2) . . ?
N4 Zr1 N1 164.7(2) . . ?
N3 Zr1 N1 88.9(2) . . ?
O2 Zr1 N2 77.0(2) . . ?
O1 Zr1 N2 91.6(2) . . ?
N4 Zr1 N2 86.3(2) . . ?
N3 Zr1 N2 167.1(2) . . ?
N1 Zr1 N2 81.6(2) . . ?
C2 O1 Zr1 142.2(4) . . ?
C16 O2 Zr1 141.2(4) . . ?
C4 N1 C6 117.4(5) . . ?
C4 N1 Zr1 129.9(4) . . ?
C6 N1 Zr1 112.6(3) . . ?
C14 N2 C18 117.5(5) . . ?
C14 N2 Zr1 128.8(4) . . ?
C18 N2 Zr1 113.5(3) . . ?
C26 N3 C25 109.7(5) . . ?
C26 N3 Zr1 123.0(4) . . ?
C25 N3 Zr1 126.9(4) . . ?
C27 N4 C28 110.0(5) . . ?
C27 N4 Zr1 125.0(4) . . ?
C28 N4 Zr1 124.2(4) . . ?
O1 C2 C3 122.8(5) . . ?
O1 C2 C1 114.3(5) . . ?
C3 C2 C1 122.8(5) . . ?
C2 C3 C4 126.2(5) . . ?
N1 C4 C3 122.4(5) . . ?
N1 C4 C5 120.7(5) . . ?
C3 C4 C5 116.9(5) . . ?
C7 C6 C11 118.4(5) . . ?
C7 C6 N1 121.0(5) . . ?
C11 C6 N1 120.5(5) . . ?
C6 C7 C8 120.9(6) . . ?
C9 C8 C7 121.0(6) . . ?
C10 C9 C8 117.3(6) . . ?
C10 C9 C12 121.6(6) . . ?
C8 C9 C12 121.1(6) . . ?
C9 C10 C11 122.3(6) . . ?
C10 C11 C6 120.1(6) . . ?
N2 C14 C15 123.3(6) . . ?
N2 C14 C13 122.8(5) . . ?
C15 C14 C13 113.9(5) . . ?
C16 C15 C14 126.2(6) . . ?
O2 C16 C15 123.0(5) . . ?
O2 C16 C17 114.9(5) . . ?
C15 C16 C17 122.0(6) . . ?
C19 C18 C23 118.1(5) . . ?
C19 C18 N2 122.1(5) . . ?
C23 C18 N2 119.7(5) . . ?
C18 C19 C20 120.6(6) . . ?
C19 C20 C21 122.6(6) . . ?
C20 C21 C22 116.5(5) . . ?
C20 C21 C24 122.8(6) . . ?
C22 C21 C24 120.6(6) . . ?
C23 C22 C21 121.7(5) . . ?
C22 C23 C18 120.5(5) . . ?
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 O2 2.050(4) . ?
Zr1 O1 2.051(4) . ?
Zr1 N4 2.077(5) . ?
Zr1 N3 2.076(5) . ?
Zr1 N1 2.385(5) . ?
Zr1 N2 2.400(5) . ?
O1 C2 1.307(6) . ?
O2 C16 1.312(7) . ?
N1 C4 1.317(7) . ?
N1 C6 1.440(7) . ?
N2 C14 1.298(7) . ?
N2 C18 1.437(7) . ?
N3 C26 1.438(7) . ?
N3 C25 1.455(7) . ?
N4 C27 1.453(7) . ?
N4 C28 1.462(7) . ?
C1 C2 1.496(8) . ?
C2 C3 1.361(8) . ?
C3 C4 1.435(8) . ?
C4 C5 1.512(8) . ?
C6 C7 1.365(8) . ?
C6 C11 1.391(7) . ?
C7 C8 1.397(8) . ?
C8 C9 1.380(8) . ?
C9 C10 1.374(9) . ?
C9 C12 1.522(8) . ?
C10 C11 1.375(8) . ?
C13 C14 1.521(8) . ?
C14 C15 1.435(7) . ?
C15 C16 1.368(8) . ?
C16 C17 1.498(7) . ?
C18 C19 1.382(8) . ?
C18 C23 1.395(7) . ?
C19 C20 1.380(8) . ?
C20 C21 1.381(8) . ?
C21 C22 1.394(8) . ?
C21 C24 1.503(8) . ?
C22 C23 1.386(7) . ?
