#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:23:19 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179325 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/22/4322271.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_4322271
loop_
_publ_author_name
'Dirk Pfeiffer'
'Bhekumusa J. Ximba'
'Louise M. Liable-Sands'
'Arnold L. Rheingold'
'Mary Jane Heeg'
'David M. Coleman'
'H. Bernhard Schlegel'
'Thomas F. Kuech'
'Charles H. Winter'
_publ_contact_author
;
     Dr. C. H. Winter
     Department of Chemistry
     Wayne State University
     Detroit, MI 48202
     USA
;
_publ_contact_author_email       cwinter@sun.science.wayne.edu
_publ_contact_author_fax         '+313 577 2099'
_publ_contact_author_phone       '+313 577 5224'
_publ_section_title
;
 Synthesis, Structure, and Molecular Orbital Studies of Yttrium, Erbium,
 and Lutetium Complexes Bearing η2-Pyrazolato Ligands: Development of a
 New Class of Precursors for Doping Semiconductors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4539
_journal_page_last               4548
_journal_paper_doi               10.1021/ic990319o
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C33 H47 Er N8'
_chemical_formula_weight         723.05
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6404(3)
_cell_length_b                   13.6404(3)
_cell_length_c                   19.1118(4)
_cell_measurement_temperature    218(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     3555.95(13)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      218(2)
_diffrn_measurement_method       'omega/phi 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  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12735
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    2.392
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       block
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(11)
_refine_ls_extinction_coef       0.0020(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.880
_refine_ls_goodness_of_fit_obs   0.889
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         4125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.370
_refine_ls_restrained_S_obs      0.889
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_obs          0.0269
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0200P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0831
_refine_ls_wR_factor_obs         0.0501
_reflns_number_observed          3577
_reflns_number_total             4130
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990319o_7.cif
_cod_data_source_block           win40
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0200P)^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^)+(0.0200P)^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_database_code               4322271
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -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
Er Er 0.174924(9) 0.174924(9) 0.0000 0.03179(7) Uani 1 d S .
N1 N 0.2134(2) 0.1787(2) 0.12072(14) 0.0428(7) Uani 1 d . .
N2 N 0.2703(2) 0.2476(2) 0.08598(14) 0.0389(7) Uani 1 d . .
N3 N 0.0355(2) 0.0831(2) 0.02706(15) 0.0361(7) Uani 1 d . .
N4 N 0.0677(2) 0.3210(2) 0.0080(2) 0.0418(6) Uani 1 d . .
C1 C 0.3303(2) 0.2893(2) 0.1326(2) 0.0400(8) Uani 1 d . .
C2 C 0.3133(3) 0.2481(3) 0.1970(2) 0.0458(9) Uani 1 d . .
H2A H 0.3454(3) 0.2636(3) 0.2391(2) 0.055 Uiso 1 calc R .
C3 C 0.2402(3) 0.1794(3) 0.1880(2) 0.0420(8) Uani 1 d . .
C4 C 0.3997(3) 0.3679(3) 0.1099(2) 0.0574(11) Uani 1 d . .
H4A H 0.3924(3) 0.3792(3) 0.0600(2) 0.086 Uiso 1 calc R .
H4B H 0.4665(3) 0.3476(3) 0.1198(2) 0.086 Uiso 1 calc R .
H4C H 0.3854(3) 0.4279(3) 0.1351(2) 0.086 Uiso 1 calc R .
C5 C 0.1906(3) 0.1141(3) 0.2406(2) 0.0673(12) Uani 1 d . .
H5A H 0.1419(3) 0.0741(3) 0.2171(2) 0.101 Uiso 1 calc R .
H5B H 0.1589(3) 0.1541(3) 0.2759(2) 0.101 Uiso 1 calc R .
H5C H 0.2390(3) 0.0721(3) 0.2626(2) 0.101 Uiso 1 calc R .
C6 C -0.0447(2) 0.0305(3) 0.0435(2) 0.0399(7) Uani 1 d . .
C7 C -0.0500(2) -0.0500(2) 0.0000 0.0465(12) Uani 1 d S .
H7A H -0.0988(2) -0.0988(2) 0.0000 0.056 Uiso 1 calc SR .
C8 C -0.1081(3) 0.0617(3) 0.1033(2) 0.0621(12) Uani 1 d . .
H8A H -0.0833(3) 0.1226(3) 0.1226(2) 0.093 Uiso 1 calc R .
H8B H -0.1074(3) 0.0114(3) 0.1392(2) 0.093 Uiso 1 calc R .
H8C H -0.1747(3) 0.0714(3) 0.0869(2) 0.093 Uiso 1 calc R .
C9 C -0.0241(3) 0.3178(3) -0.0166(2) 0.0491(9) Uani 1 d . .
H9A H -0.0492(3) 0.2570(3) -0.0312(2) 0.059 Uiso 1 calc R .
C10 C -0.0837(3) 0.3990(3) -0.0216(2) 0.0503(10) Uani 1 d . .
H10A H -0.1469(3) 0.3922(3) -0.0407(2) 0.060 Uiso 1 calc R .
C11 C -0.0527(2) 0.4900(2) 0.0009(2) 0.0422(8) Uani 1 d . .
C12 C 0.0428(3) 0.4935(3) 0.0265(2) 0.0534(11) Uani 1 d . .
H12A H 0.0696(3) 0.5534(3) 0.0416(2) 0.064 Uiso 1 calc R .
C13 C 0.0981(3) 0.4089(3) 0.0297(2) 0.0544(11) Uani 1 d . .
H13A H 0.1616(3) 0.4135(3) 0.0484(2) 0.065 Uiso 1 calc R .
C14 C -0.1161(3) 0.5818(3) -0.0042(3) 0.0521(9) Uani 1 d . .
C15 C -0.2229(3) 0.5558(4) -0.0111(4) 0.105(2) Uani 1 d . .
H15A H -0.2430(3) 0.5172(4) 0.0291(4) 0.158 Uiso 1 calc R .
H15B H -0.2328(3) 0.5180(4) -0.0535(4) 0.158 Uiso 1 calc R .
H15C H -0.2616(3) 0.6153(4) -0.0132(4) 0.158 Uiso 1 calc R .
C16 C -0.1048(5) 0.6452(4) 0.0617(3) 0.094(2) Uani 1 d . .
H16A H -0.0365(5) 0.6632(4) 0.0676(3) 0.141 Uiso 1 calc R .
H16B H -0.1266(5) 0.6084(4) 0.1022(3) 0.141 Uiso 1 calc R .
H16C H -0.1442(5) 0.7040(4) 0.0569(3) 0.141 Uiso 1 calc R .
C17 C -0.0832(5) 0.6418(4) -0.0662(3) 0.118(3) Uani 1 d . .
H17A H -0.0143(5) 0.6580(4) -0.0611(3) 0.176 Uiso 1 calc R .
H17B H -0.1214(5) 0.7017(4) -0.0686(3) 0.176 Uiso 1 calc R .
H17C H -0.0927(5) 0.6043(4) -0.1088(3) 0.176 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'
Er Er -0.2586 4.9576 '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
N2 Er N2 91.28(13) . 7 ?
N2 Er N3 143.73(10) . 7 ?
N2 Er N3 121.96(9) 7 7 ?
N2 Er N3 121.96(9) . . ?
N2 Er N3 143.73(10) 7 . ?
N3 Er N3 34.45(13) 7 . ?
N2 Er N1 125.71(10) . 7 ?
N2 Er N1 34.44(9) 7 7 ?
N3 Er N1 88.65(10) 7 7 ?
N3 Er N1 110.65(10) . 7 ?
N2 Er N1 34.44(9) . . ?
N2 Er N1 125.71(10) 7 . ?
N3 Er N1 110.65(10) 7 . ?
N3 Er N1 88.65(9) . . ?
N1 Er N1 160.15(13) 7 . ?
N2 Er N4 86.79(10) . . ?
N2 Er N4 81.08(10) 7 . ?
N3 Er N4 110.60(9) 7 . ?
N3 Er N4 86.37(9) . . ?
N1 Er N4 83.93(10) 7 . ?
N1 Er N4 93.08(10) . . ?
N2 Er N4 81.07(10) . 7 ?
N2 Er N4 86.78(10) 7 7 ?
N3 Er N4 86.38(9) 7 7 ?
N3 Er N4 110.60(9) . 7 ?
N1 Er N4 93.08(10) 7 7 ?
N1 Er N4 83.93(10) . 7 ?
N4 Er N4 162.62(12) . 7 ?
C3 N1 N2 107.6(3) . . ?
C3 N1 Er 176.9(2) . . ?
N2 N1 Er 70.9(2) . . ?
C1 N2 N1 108.2(3) . . ?
C1 N2 Er 176.2(2) . . ?
N1 N2 Er 74.7(2) . . ?
C6 N3 N3 107.8(2) . 7 ?
C6 N3 Er 179.3(2) . . ?
N3 N3 Er 72.78(6) 7 . ?
C13 N4 C9 115.4(3) . . ?
C13 N4 Er 123.9(2) . . ?
C9 N4 Er 120.4(2) . . ?
N2 C1 C2 108.6(3) . . ?
N2 C1 C4 120.0(3) . . ?
C2 C1 C4 131.4(3) . . ?
C1 C2 C3 106.8(3) . . ?
N1 C3 C2 108.8(3) . . ?
N1 C3 C5 121.0(4) . . ?
C2 C3 C5 130.2(3) . . ?
N3 C6 C7 109.2(3) . . ?
N3 C6 C8 119.7(3) . . ?
C7 C6 C8 131.0(4) . . ?
C6 C7 C6 106.1(4) 7 . ?
N4 C9 C10 123.4(3) . . ?
C9 C10 C11 121.4(3) . . ?
C10 C11 C12 115.3(3) . . ?
C10 C11 C14 123.0(3) . . ?
C12 C11 C14 121.7(3) . . ?
C13 C12 C11 119.9(3) . . ?
N4 C13 C12 124.6(4) . . ?
C15 C14 C17 110.4(5) . . ?
C15 C14 C11 111.1(3) . . ?
C17 C14 C11 109.1(3) . . ?
C15 C14 C16 107.5(4) . . ?
C17 C14 C16 108.0(4) . . ?
C11 C14 C16 110.7(4) . . ?
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
Er N2 2.319(3) . ?
Er N2 2.319(3) 7 ?
Er N3 2.335(3) 7 ?
Er N3 2.335(3) . ?
Er N1 2.367(3) 7 ?
Er N1 2.367(3) . ?
Er N4 2.476(3) . ?
Er N4 2.476(3) 7 ?
N1 C3 1.337(4) . ?
N1 N2 1.388(4) . ?
N2 C1 1.337(4) . ?
N3 C6 1.345(5) . ?
N3 N3 1.383(5) 7 ?
N4 C13 1.335(4) . ?
N4 C9 1.338(4) . ?
C1 C2 1.373(5) . ?
C1 C4 1.495(5) . ?
C2 C3 1.379(5) . ?
C3 C5 1.503(6) . ?
C6 C7 1.379(4) . ?
C6 C8 1.496(5) . ?
C7 C6 1.379(4) 7 ?
C9 C10 1.377(5) . ?
C10 C11 1.380(5) . ?
C11 C12 1.393(5) . ?
C11 C14 1.524(5) . ?
C12 C13 1.380(5) . ?
C14 C15 1.505(6) . ?
C14 C17 1.509(6) . ?
C14 C16 1.536(6) . ?
