#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:41:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179419 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/16/4331629.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_4331629
loop_
_publ_author_name
'Cortés-Llamas, Sara-Ángelica'
'Hernández-Lamoneda, Ramón'
'Velázquez-Carmona, Miguel-Ángel'
'Muñoz-Hernández, Miguel-Angel'
'Toscano, Rubén A.'
_publ_section_title
;
 3,5-Dimethyl and 3,5-Di-tert-butylpyrazolato Complexes with Alkali
 Metals:  Monomeric, Dimeric, Cluster, and 1D Chain Structures
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              286
_journal_page_last               294
_journal_paper_doi               10.1021/ic051294y
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C44 H78 Li2 N8'
_chemical_formula_weight         733.02
_chemical_name_systematic
; 
(3,5-di-tert-butylpyrazole)(3,5-di-tert-butylpyrazolato)lithium 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.982(5)
_cell_angle_beta                 71.500(4)
_cell_angle_gamma                75.143(5)
_cell_formula_units_Z            2
_cell_length_a                   10.310(3)
_cell_length_b                   10.826(3)
_cell_length_c                   11.412(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1167.2(6)
_computing_cell_refinement       'SMART V 5.625 (Bruker, 1999)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'SAINT V 6.23C (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL V 6.10 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V 6.10 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL V 6.10 (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL V 6.10 (Sheldrick, 2000)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0.661
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer'
_diffrn_measurement_method       ω-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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7049
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.043
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.150
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0490P)²+0.3442P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                3078
_reflns_number_total             4057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051294ysup2.cif
_cod_data_source_block           Compound_2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_database_code               4331629
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Li1 Li1 0.1122(4) 0.4355(4) 0.9226(4) 0.0273(9) Uani 1 1 d .
N1 N 0.0793(2) 0.33293(17) 1.08211(17) 0.0205(5) Uani 1 1 d .
N2 N -0.0480(2) 0.37314(17) 1.05649(17) 0.0208(5) Uani 1 1 d .
N3 N 0.1882(2) 0.41167(18) 0.73542(17) 0.0260(5) Uani 1 1 d .
N4 N 0.1817(2) 0.52356(19) 0.66777(19) 0.0274(5) Uani 1 1 d .
H4 H 0.144(3) 0.597(3) 0.708(2) 0.041 Uiso 1 1 d .
C1 C 0.0785(2) 0.2223(2) 1.14680(19) 0.0191(5) Uani 1 1 d .
C2 C -0.0478(2) 0.1888(2) 1.1640(2) 0.0212(5) Uani 1 1 d .
H2 H -0.0760 0.1154 1.2068 0.025 Uiso 1 1 calc R
C3 C -0.1243(2) 0.2859(2) 1.1050(2) 0.0211(5) Uani 1 1 d .
C4 C 0.2045(3) 0.1544(2) 1.1899(2) 0.0237(5) Uani 1 1 d .
C5 C 0.1763(3) 0.0349(2) 1.2678(2) 0.0345(7) Uani 1 1 d .
H5A H 0.0948 0.0595 1.3410 0.052 Uiso 1 1 calc R
H5B H 0.2590 -0.0081 1.2938 0.052 Uiso 1 1 calc R
H5C H 0.1569 -0.0232 1.2187 0.052 Uiso 1 1 calc R
C6 C 0.3350(3) 0.1165(3) 1.0783(2) 0.0334(6) Uani 1 1 d .
H6A H 0.3177 0.0597 1.0264 0.050 Uiso 1 1 calc R
H6B H 0.4155 0.0721 1.1068 0.050 Uiso 1 1 calc R
H6C H 0.3554 0.1934 1.0301 0.050 Uiso 1 1 calc R
C7 C 0.2330(3) 0.2455(2) 1.2676(2) 0.0323(6) Uani 1 1 d .
H7A H 0.2519 0.3219 1.2177 0.049 Uiso 1 1 calc R
H7B H 0.3147 0.2026 1.2950 0.049 Uiso 1 1 calc R
H7C H 0.1504 0.2704 1.3399 0.049 Uiso 1 1 calc R
C8 C -0.2674(3) 0.3000(2) 1.0882(2) 0.0276(6) Uani 1 1 d .
C9 C -0.3668(3) 0.2540(3) 1.2041(2) 0.0365(7) Uani 1 1 d .
H9A H -0.3250 0.1656 1.2242 0.055 Uiso 1 1 calc R
H9B H -0.4567 0.2582 1.1898 0.055 Uiso 1 1 calc R
H9C H -0.3828 0.3086 1.2730 0.055 Uiso 1 1 calc R
C10 C -0.3319(3) 0.4390(3) 1.0604(3) 0.0444(8) Uani 1 1 d .
H10A H -0.3426 0.4919 1.1291 0.067 Uiso 1 1 calc R
H10B H -0.4243 0.4456 1.0502 0.067 Uiso 1 1 calc R
H10C H -0.2701 0.4687 0.9842 0.067 Uiso 1 1 calc R
C11 C -0.2484(3) 0.2166(3) 0.9797(3) 0.0480(8) Uani 1 1 d .
H11A H -0.1881 0.2480 0.9036 0.072 Uiso 1 1 calc R
H11B H -0.3404 0.2210 0.9698 0.072 Uiso 1 1 calc R
H11C H -0.2045 0.1278 0.9968 0.072 Uiso 1 1 calc R
C12 C 0.2504(2) 0.3203(2) 0.6513(2) 0.0224(5) Uani 1 1 d .
C13 C 0.2842(2) 0.3761(2) 0.5325(2) 0.0236(5) Uani 1 1 d .
H13 H 0.3302 0.3321 0.4571 0.028 Uiso 1 1 calc R
C14 C 0.2387(2) 0.5058(2) 0.5451(2) 0.0228(5) Uani 1 1 d .
C15 C 0.2377(3) 0.6136(2) 0.4493(2) 0.0278(6) Uani 1 1 d .
C16 C 0.1134(3) 0.6243(3) 0.4001(3) 0.0453(8) Uani 1 1 d .
H16A H 0.1224 0.5432 0.3639 0.068 Uiso 1 1 calc R
H16B H 0.1127 0.6928 0.3368 0.068 Uiso 1 1 calc R
H16C H 0.0253 0.6439 0.4681 0.068 Uiso 1 1 calc R
C17 C 0.2252(4) 0.7400(2) 0.5044(3) 0.0507(9) Uani 1 1 d .
H17A H 0.1391 0.7590 0.5745 0.076 Uiso 1 1 calc R
H17B H 0.2216 0.8086 0.4414 0.076 Uiso 1 1 calc R
H17C H 0.3070 0.7337 0.5328 0.076 Uiso 1 1 calc R
C18 C 0.3743(3) 0.5820(3) 0.3432(2) 0.0371(7) Uani 1 1 d .
H18A H 0.4545 0.5726 0.3746 0.056 Uiso 1 1 calc R
H18B H 0.3749 0.6511 0.2804 0.056 Uiso 1 1 calc R
H18C H 0.3813 0.5018 0.3063 0.056 Uiso 1 1 calc R
C19 C 0.2791(3) 0.1799(2) 0.6892(2) 0.0244(6) Uani 1 1 d .
C20 C 0.2861(4) 0.0999(2) 0.5833(2) 0.0464(8) Uani 1 1 d .
H20A H 0.1962 0.1250 0.5648 0.070 Uiso 1 1 calc R
H20B H 0.3045 0.0091 0.6078 0.070 Uiso 1 1 calc R
H20C H 0.3619 0.1145 0.5098 0.070 Uiso 1 1 calc R
C21 C 0.4204(3) 0.1412(3) 0.7159(3) 0.0434(8) Uani 1 1 d .
H21A H 0.4954 0.1543 0.6410 0.065 Uiso 1 1 calc R
H21B H 0.4386 0.0509 0.7419 0.065 Uiso 1 1 calc R
H21C H 0.4178 0.1937 0.7819 0.065 Uiso 1 1 calc R
C22 C 0.1620(3) 0.1543(2) 0.8037(2) 0.0338(7) Uani 1 1 d .
H22A H 0.1583 0.2031 0.8728 0.051 Uiso 1 1 calc R
H22B H 0.1810 0.0628 0.8255 0.051 Uiso 1 1 calc R
H22C H 0.0715 0.1804 0.7862 0.051 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'
Li Li -0.0003 0.0001 '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'
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
N1 Li1 N2 114.3(2) . 2_567
N1 Li1 N3 140.8(2) . .
N2 Li1 N3 104.89(18) 2_567 .
N1 Li1 N2 39.73(10) . .
N2 Li1 N2 101.53(18) 2_567 .
N3 Li1 N2 131.4(2) . .
N1 Li1 Li1 73.00(18) . 2_567
N2 Li1 Li1 51.54(14) 2_567 2_567
N3 Li1 Li1 136.8(3) . 2_567
N2 Li1 Li1 49.99(14) . 2_567
C1 N1 N2 107.58(18) . .
C1 N1 Li1 152.30(19) . .
N2 N1 Li1 72.38(16) . .
C3 N2 N1 108.28(17) . .
C3 N2 Li1 127.10(19) . 2_567
N1 N2 Li1 107.41(18) . 2_567
C3 N2 Li1 152.00(19) . .
N1 N2 Li1 67.89(16) . .
Li1 N2 Li1 78.47(18) 2_567 .
C12 N3 N4 104.67(18) . .
C12 N3 Li1 141.28(19) . .
N4 N3 Li1 113.97(18) . .
C14 N4 N3 112.96(19) . .
N1 C1 C2 109.8(2) . .
N1 C1 C4 120.1(2) . .
C2 C1 C4 130.1(2) . .
C1 C2 C3 105.4(2) . .
N2 C3 C2 108.9(2) . .
N2 C3 C8 121.06(19) . .
C2 C3 C8 130.0(2) . .
C1 C4 C5 110.7(2) . .
C1 C4 C6 109.97(19) . .
C5 C4 C6 109.4(2) . .
C1 C4 C7 109.08(19) . .
C5 C4 C7 109.3(2) . .
C6 C4 C7 108.4(2) . .
C3 C8 C9 110.4(2) . .
C3 C8 C10 111.0(2) . .
C9 C8 C10 108.8(2) . .
C3 C8 C11 108.1(2) . .
C9 C8 C11 108.8(2) . .
C10 C8 C11 109.7(2) . .
N3 C12 C13 109.8(2) . .
N3 C12 C19 121.5(2) . .
C13 C12 C19 128.7(2) . .
C14 C13 C12 107.3(2) . .
N4 C14 C13 105.3(2) . .
N4 C14 C15 123.6(2) . .
C13 C14 C15 131.0(2) . .
C14 C15 C17 111.1(2) . .
C14 C15 C18 108.7(2) . .
C17 C15 C18 109.4(2) . .
C14 C15 C16 108.7(2) . .
C17 C15 C16 109.8(2) . .
C18 C15 C16 109.1(2) . .
C12 C19 C21 109.2(2) . .
C12 C19 C22 110.60(19) . .
C21 C19 C22 110.0(2) . .
C12 C19 C20 109.42(19) . .
C21 C19 C20 108.9(2) . .
C22 C19 C20 108.7(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Li1 N1 2.009(4) .
Li1 N2 2.022(4) 2_567
Li1 N3 2.048(4) .
Li1 N2 2.067(4) .
Li1 Li1 2.586(8) 2_567
N1 C1 1.340(3) .
N1 N2 1.386(3) .
N2 C3 1.347(3) .
N2 Li1 2.022(4) 2_567
N3 C12 1.340(3) .
N3 N4 1.365(3) .
N4 C14 1.348(3) .
C1 C2 1.389(3) .
C1 C4 1.520(3) .
C2 C3 1.393(3) .
C3 C8 1.515(3) .
C4 C5 1.528(3) .
C4 C6 1.530(3) .
C4 C7 1.531(3) .
C8 C9 1.520(3) .
C8 C10 1.526(4) .
C8 C11 1.540(4) .
C12 C13 1.401(3) .
C12 C19 1.515(3) .
C13 C14 1.369(3) .
C14 C15 1.514(3) .
C15 C17 1.525(3) .
C15 C18 1.525(3) .
C15 C16 1.529(4) .
C19 C21 1.527(4) .
C19 C22 1.529(3) .
C19 C20 1.532(3) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4 N2 0.89(3) 2.57(3) 3.201(3) 128(2) 2_567
