#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:38:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179339 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/36/4323696.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_4323696
loop_
_publ_author_name
'Karl Weis'
'Heinrich Vahrenkamp'
_publ_section_title
;
 Simple Zinc Complexes of Pyridyl-Substituted Tris(pyrazolyl)borate
 Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5592
_journal_page_last               5596
_journal_paper_doi               10.1021/ic970628j
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        Ethanol
_chemical_formula_sum            'C29 H31 B I N9 O Zn'
_chemical_formula_weight         724.71
_chemical_melting_point          261
_chemical_name_systematic
Hydrotris(5-methyl-3-3'-pyridyl-pyrazole-1-yl)borato-zinc-iodide
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 101.99(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.922(1)
_cell_length_b                   10.476(4)
_cell_length_c                   31.444(1)
_cell_measurement_temperature    293(2)
_cell_volume                     6097(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nonius-Turbo CAD4'
_diffrn_measurement_method       Omega-2Theta
_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  0.0138
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            6097
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.39
_diffrn_standards_interval_count 'ICR every 3600s, OCR every 200 refl.'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.858
_exptl_absorpt_correction_T_max  0.655
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   'empirical (XEMP)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_meas      1.52
_exptl_crystal_description       isometric
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.071
_refine_ls_goodness_of_fit_obs   1.044
_refine_ls_hydrogen_treatment    Riding-Model
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.044
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_obs          0.0337
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0567P)²+9.2828P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1023
_refine_ls_wR_factor_obs         0.0896
_reflns_number_observed          4963
_reflns_number_total             5980
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970628j_1.cif
_cod_data_source_block           w29
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (50 times).

'_geom_angle_publ_flag' value 'Y'
changed to 'y' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (80
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+9.2828P] 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^)+(0.0567P)^2^+9.2828P] 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        6097.1(5)
_cod_database_code               4323696
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Zn Zn 0.51316(2) -0.07681(4) 0.373582(13) 0.04638(11) Uani 1 d . .
N1 N 0.47023(14) -0.2003(2) 0.41154(8) 0.0403(5) Uani 1 d . .
N2 N 0.60555(14) -0.1792(3) 0.37283(8) 0.0431(6) Uani 1 d . .
N3 N 0.4550(2) -0.1780(3) 0.31890(9) 0.0476(6) Uani 1 d . .
I I 0.500061(14) 0.15939(2) 0.361987(8) 0.05630(10) Uani 1 d . .
N4 N 0.48408(14) -0.3258(2) 0.40316(8) 0.0411(6) Uani 1 d . .
C1 C 0.4637(2) -0.4026(3) 0.43286(10) 0.0436(7) Uani 1 d . .
C2 C 0.4371(2) -0.3256(3) 0.46131(10) 0.0452(7) Uani 1 d . .
H2 H 0.4197(2) -0.3517(3) 0.48548(10) 0.054 Uiso 1 calc R .
C3 C 0.4413(2) -0.2017(3) 0.44693(9) 0.0400(6) Uani 1 d . .
C4 C 0.4695(2) -0.5443(3) 0.43175(12) 0.0583(9) Uani 1 d . .
H4A H 0.4558(2) -0.5799(3) 0.45699(12) 0.087 Uiso 1 calc R .
H4B H 0.5184(2) -0.5679(3) 0.43150(12) 0.087 Uiso 1 calc R .
H4C H 0.4380(2) -0.5764(3) 0.40604(12) 0.087 Uiso 1 calc R .
C5 C 0.4197(2) -0.0840(3) 0.46663(10) 0.0412(6) Uani 1 d . .
C6 C 0.4274(2) -0.0791(3) 0.51174(11) 0.0459(7) Uani 1 d . .
H6 H 0.4440(2) -0.1518(3) 0.52771(11) 0.055 Uiso 1 calc R .
N7 N 0.4124(2) 0.0239(3) 0.53330(10) 0.0536(7) Uani 1 d . .
C7 C 0.3879(2) 0.1263(4) 0.50940(14) 0.0593(9) Uani 1 d . .
H7 H 0.3777(2) 0.1994(4) 0.52379(14) 0.071 Uiso 1 calc R .
C8 C 0.3769(2) 0.1301(4) 0.46479(14) 0.0582(9) Uani 1 d . .
H8 H 0.3587(2) 0.2032(4) 0.44959(14) 0.070 Uiso 1 calc R .
C9 C 0.3935(2) 0.0235(3) 0.44304(12) 0.0516(8) Uani 1 d . .
H9 H 0.3870(2) 0.0239(3) 0.41291(12) 0.062 Uiso 1 calc R .
N5 N 0.59231(15) -0.3078(3) 0.36717(9) 0.0453(6) Uani 1 d . .
C10 C 0.6526(2) -0.3675(3) 0.36065(11) 0.0509(8) Uani 1 d . .
C11 C 0.7052(2) -0.2772(4) 0.36223(11) 0.0536(8) Uani 1 d . .
H11 H 0.7523(2) -0.2909(4) 0.35885(11) 0.064 Uiso 1 calc R .
C12 C 0.6746(2) -0.1607(3) 0.36991(10) 0.0451(7) Uani 1 d . .
C13 C 0.6558(3) -0.5078(4) 0.35240(15) 0.0716(11) Uani 1 d . .
H13A H 0.7030(3) -0.5298(4) 0.34808(15) 0.107 Uiso 1 calc R .
H13B H 0.6204(3) -0.5297(4) 0.32689(15) 0.107 Uiso 1 calc R .
H13C H 0.6460(3) -0.5539(4) 0.37692(15) 0.107 Uiso 1 calc R .
C14 C 0.7097(2) -0.0350(3) 0.37370(10) 0.0460(7) Uani 1 d . .
C15 C 0.6910(2) 0.0616(4) 0.39894(11) 0.0509(8) Uani 1 d . .
H15 H 0.6544(2) 0.0452(4) 0.41391(11) 0.061 Uiso 1 calc R .
N8 N 0.7215(2) 0.1768(3) 0.40347(11) 0.0596(8) Uani 1 d . .
C16 C 0.7739(2) 0.1983(4) 0.38232(13) 0.0636(10) Uani 1 d . .
H16 H 0.7960(2) 0.2780(4) 0.38509(13) 0.076 Uiso 1 calc R .
C17 C 0.7973(2) 0.1088(5) 0.3565(2) 0.0730(12) Uani 1 d . .
H17 H 0.8345(2) 0.1278(5) 0.3424(2) 0.088 Uiso 1 calc R .
C18 C 0.7651(2) -0.0088(4) 0.35191(13) 0.0632(10) Uani 1 d . .
H18 H 0.7801(2) -0.0706(4) 0.33444(13) 0.076 Uiso 1 calc R .
N6 N 0.4664(2) -0.3068(3) 0.32181(8) 0.0471(6) Uani 1 d . .
C19 C 0.4285(2) -0.3657(4) 0.28627(11) 0.0555(9) Uani 1 d . .
C20 C 0.3925(2) -0.2727(5) 0.25961(12) 0.0657(10) Uani 1 d . .
H20 H 0.3624(2) -0.2846(5) 0.23249(12) 0.079 Uiso 1 calc R .
C21 C 0.4096(2) -0.1570(4) 0.28101(11) 0.0515(8) Uani 1 d . .
C22 C 0.4262(3) -0.5073(5) 0.28124(15) 0.0811(13) Uani 1 d . .
H22A H 0.3959(3) -0.5294(5) 0.25379(15) 0.122 Uiso 1 calc R .
H22B H 0.4071(3) -0.5448(5) 0.30434(15) 0.122 Uiso 1 calc R .
H22C H 0.4742(3) -0.5390(5) 0.28237(15) 0.122 Uiso 1 calc R .
C23 C 0.3801(2) -0.0291(4) 0.26849(11) 0.0532(9) Uani 1 d . .
C24 C 0.3976(2) 0.0398(4) 0.23506(12) 0.0613(9) Uani 1 d . .
H24 H 0.4306(2) 0.0074(4) 0.21965(12) 0.074 Uiso 1 calc R .
N9 N 0.3659(3) 0.1584(4) 0.2243(2) 0.0959(13) Uani 1 d . .
C25 C 0.3164(3) 0.2002(5) 0.2482(2) 0.0806(13) Uani 1 d . .
H25 H 0.2940(3) 0.2786(5) 0.2410(2) 0.097 Uiso 1 calc R .
C26 C 0.2995(2) 0.1358(5) 0.2800(2) 0.0784(13) Uani 1 d . .
H26 H 0.2663(2) 0.1675(5) 0.2954(2) 0.094 Uiso 1 calc R .
C27 C 0.3304(2) 0.0254(5) 0.28968(15) 0.0817(14) Uani 1 d . .
H27 H 0.3182(2) -0.0201(5) 0.31252(15) 0.098 Uiso 1 calc R .
B B 0.5156(2) -0.3629(4) 0.36307(12) 0.0448(8) Uiso 1 d . .
H0 H 0.5172(2) -0.4561(4) 0.36065(12) 0.054 Uiso 1 calc R .
O O 0.6581(2) 0.3536(3) 0.45561(11) 0.0756(8) Uani 1 d . .
H1O H 0.6898(2) 0.2655(3) 0.42959(11) 0.113 Uiso 1 d R .
C28 C 0.7155(2) 0.4257(5) 0.4784(2) 0.0833(14) Uani 1 d . .
H28A H 0.7507(2) 0.4381(5) 0.4604(2) 0.100 Uiso 1 calc R .
H28B H 0.7388(2) 0.3792(5) 0.5042(2) 0.100 Uiso 1 calc R .
C29 C 0.6920(3) 0.5494(5) 0.4912(2) 0.099(2) Uani 1 d . .
H29A H 0.7328(3) 0.5949(5) 0.5075(2) 0.148 Uiso 1 calc R .
H29B H 0.6567(3) 0.5376(5) 0.5088(2) 0.148 Uiso 1 calc R .
H29C H 0.6711(3) 0.5974(5) 0.4656(2) 0.148 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'
B B 0.0013 0.0007 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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 Zn N2 96.81(10) . . y
N1 Zn N3 87.42(10) . . y
N2 Zn N3 91.64(11) . . y
N1 Zn I 132.23(7) . . y
N2 Zn I 124.92(8) . . y
N3 Zn I 110.87(8) . . y
N1 Zn N7 73.25(9) . 5_656 y
N2 Zn N7 83.15(9) . 5_656 y
N3 Zn N7 159.14(9) . 5_656 y
I Zn N7 88.40(6) . 5_656 y
C3 N1 N4 106.0(2) . . y
C3 N1 Zn 140.8(2) . . y
N4 N1 Zn 112.3(2) . . y
C12 N2 N5 106.6(3) . . y
C12 N2 Zn 140.1(2) . . y
N5 N2 Zn 112.4(2) . . y
C21 N3 N6 106.6(3) . . y
C21 N3 Zn 140.4(3) . . y
N6 N3 Zn 113.0(2) . . y
C1 N4 N1 110.1(2) . . y
C1 N4 B 128.8(3) . . y
N1 N4 B 121.0(2) . . y
N4 C1 C2 107.2(3) . . y
N4 C1 C4 123.0(3) . . y
C2 C1 C4 129.7(3) . . y
C1 C2 C3 106.5(3) . . y
N1 C3 C2 110.1(3) . . y
N1 C3 C5 122.5(3) . . y
C2 C3 C5 127.4(3) . . y
C9 C5 C6 117.7(3) . . y
C9 C5 C3 123.7(3) . . y
C6 C5 C3 118.6(3) . . y
N7 C6 C5 123.9(3) . . y
C6 N7 C7 116.6(3) . . y
N7 C7 C8 123.9(3) . . y
C7 C8 C9 118.7(4) . . y
C8 C9 C5 119.1(3) . . y
C10 N5 N2 109.7(3) . . y
C10 N5 B 128.4(3) . . y
N2 N5 B 121.4(3) . . y
N5 C10 C11 107.7(3) . . y
N5 C10 C13 123.2(4) . . y
C11 C10 C13 129.1(3) . . y
C10 C11 C12 106.6(3) . . y
N2 C12 C11 109.4(3) . . y
N2 C12 C14 123.6(3) . . y
C11 C12 C14 127.0(3) . . y
C15 C14 C18 116.7(3) . . y
C15 C14 C12 122.6(3) . . y
C18 C14 C12 120.7(3) . . y
N8 C15 C14 124.7(3) . . y
C16 N8 C15 116.9(3) . . y
C16 N8 O 128.2(3) . . y
C15 N8 O 114.8(2) . . y
N8 C16 C17 123.3(4) . . y
C18 C17 C16 119.2(4) . . y
C17 C18 C14 119.2(4) . . y
C19 N6 N3 110.4(3) . . y
C19 N6 B 130.2(3) . . y
N3 N6 B 119.4(3) . . y
N6 C19 C20 107.1(3) . . y
N6 C19 C22 122.9(4) . . y
C20 C19 C22 130.0(4) . . y
C19 C20 C21 106.7(3) . . y
N3 C21 C20 109.3(3) . . y
N3 C21 C23 121.8(3) . . y
C20 C21 C23 128.7(3) . . y
C27 C23 C24 116.6(4) . . y
C27 C23 C21 120.3(4) . . y
C24 C23 C21 123.1(3) . . y
N9 C24 C23 119.8(4) . . y
C24 N9 C25 117.1(4) . . y
C26 C25 N9 123.7(5) . . y
C27 C26 C25 118.0(4) . . y
C26 C27 C23 124.8(4) . . y
N5 B N4 110.6(3) . . y
N5 B N6 108.6(3) . . y
N4 B N6 108.7(3) . . y
C28 O N8 105.6(3) . . y
O C28 C29 112.1(4) . . y
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
Zn N1 2.040(3) . y
Zn N2 2.056(3) . y
Zn N3 2.122(3) . y
Zn I 2.506(4) . y
Zn N7 3.025(3) 5_656 y
N1 C3 1.338(4) . y
N1 N4 1.376(4) . y
N2 C12 1.342(4) . y
N2 N5 1.374(4) . y
N3 C21 1.335(4) . y
N3 N6 1.366(4) . y
N4 C1 1.349(4) . y
N4 B 1.552(4) . y
C1 C2 1.375(5) . y
C1 C4 1.489(5) . y
C2 C3 1.382(5) . y
C3 C5 1.475(4) . y
C5 C9 1.383(5) . y
C5 C6 1.396(4) . y
C6 N7 1.336(4) . y
N7 C7 1.336(5) . y
C7 C8 1.375(6) . y
C8 C9 1.379(5) . y
N5 C10 1.353(4) . y
N5 B 1.543(5) . y
C10 C11 1.368(5) . y
C10 C13 1.495(5) . y
C11 C12 1.393(5) . y
C12 C14 1.469(5) . y
C14 C15 1.377(5) . y
C14 C18 1.394(5) . y
C15 N8 1.333(5) . y
N8 C16 1.324(5) . y
N8 O 2.894(4) . y
C16 C17 1.371(7) . y
C17 C18 1.369(6) . y
N6 C19 1.346(4) . y
N6 B 1.547(5) . y
C19 C20 1.371(6) . y
C19 C22 1.492(6) . y
C20 C21 1.392(6) . y
C21 C23 1.472(5) . y
C23 C27 1.384(6) . y
C23 C24 1.372(5) . y
C24 N9 1.390(6) . y
N9 C25 1.389(7) . y
C25 C26 1.300(7) . y
C26 C27 1.304(7) . y
O C28 1.393(5) . y
C28 C29 1.453(6) . y
