#------------------------------------------------------------------------------
#$Date: 2024-11-15 14:46:36 +0200 (Fri, 15 Nov 2024) $
#$Revision: 295934 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/15/4311573.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_4311573
loop_
_publ_author_name
'Horst Brombacher'
'Heinrich Vahrenkamp'
_publ_section_title
;
 Pyrazolylborate-Zinc Alkoxide Complexes. 3. Acid-Base Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6054
_journal_page_last               6060
_journal_paper_doi               10.1021/ic049177a
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C34 H30 B N8 Zn'
_chemical_formula_weight         626.84
_chemical_melting_point          232
_chemical_name_common            Tp(Ph,Me)ZnCH2CN
_chemical_name_systematic
; 
 Hydrotris(3-phenyl-5-methylpyrazol-1-yl)borato-zink-cyanomethanid 
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.720(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4868(13)
_cell_length_b                   25.565(3)
_cell_length_c                   10.8602(11)
_cell_measurement_temperature    294(2)
_cell_volume                     3149.2(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0938
_diffrn_reflns_av_sigmaI/netI    0.1091
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28458
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       isometric
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       0.023(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         7653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1782
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          1.970
_refine_ls_shift/su_mean         0.053
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1370P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.2610
_reflns_number_gt                3287
_reflns_number_total             7653
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049177asi20040706_093708_6.cif
_cod_data_source_block           brombk2
_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.

'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (75
times).

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (50 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4311573
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
Zn1 Zn 0.27820(6) 0.62406(2) 0.30687(6) 0.0491(3) Uani 1 1 d . . .
N1 N 0.1095(4) 0.63872(19) 0.2904(5) 0.0546(12) Uani 1 1 d . . .
N2 N 0.2794(4) 0.55213(17) 0.3947(4) 0.0508(11) Uani 1 1 d . . .
N3 N 0.3567(4) 0.65981(18) 0.4951(4) 0.0514(11) Uani 1 1 d . . .
N4 N 0.0931(4) 0.62223(18) 0.4013(5) 0.0507(11) Uani 1 1 d . . .
N5 N 0.2577(4) 0.55734(17) 0.5092(4) 0.0510(11) Uani 1 1 d . . .
N6 N 0.2918(4) 0.65242(18) 0.5704(4) 0.0498(11) Uani 1 1 d . . .
N7 N 0.5135(8) 0.6047(3) 0.1651(9) 0.116(3) Uani 1 1 d . . .
N8 N 0.136(4) 0.5962(19) -0.162(5) 0.66(3) Uiso 1 1 d U . .
B1 B 0.2023(6) 0.6080(3) 0.5340(7) 0.0512(15) Uani 1 1 d . . .
H1B H 0.165(4) 0.5998(18) 0.608(5) 0.040(13) Uiso 1 1 d . . .
C1 C -0.0238(5) 0.6183(2) 0.3711(6) 0.0592(15) Uani 1 1 d . . .
C2 C -0.0836(6) 0.6319(3) 0.2367(7) 0.0721(19) Uani 1 1 d . . .
H2A H -0.1648 0.6320 0.1860 0.086 Uiso 1 1 calc R . .
C3 C 0.0013(5) 0.6452(2) 0.1925(6) 0.0565(14) Uani 1 1 d . . .
C4 C -0.0674(7) 0.6020(4) 0.4752(8) 0.095(2) Uani 1 1 d . . .
H4A H -0.0013 0.5958 0.5603 0.142 Uiso 1 1 calc R . .
H4B H -0.1129 0.5705 0.4459 0.142 Uiso 1 1 calc R . .
H4C H -0.1158 0.6292 0.4859 0.142 Uiso 1 1 calc R . .
C5 C -0.0164(5) 0.6651(2) 0.0558(6) 0.0589(15) Uani 1 1 d . . .
C6 C -0.1034(6) 0.6455(3) -0.0618(7) 0.0748(19) Uani 1 1 d . . .
H6A H -0.1503 0.6180 -0.0570 0.090 Uiso 1 1 calc R . .
C7 C -0.1222(8) 0.6664(4) -0.1882(7) 0.092(2) Uani 1 1 d . . .
H7A H -0.1818 0.6528 -0.2662 0.110 Uiso 1 1 calc R . .
C8 C -0.0554(8) 0.7057(4) -0.1984(8) 0.095(3) Uani 1 1 d . . .
H8A H -0.0686 0.7194 -0.2830 0.114 Uiso 1 1 calc R . .
C9 C 0.0331(8) 0.7260(3) -0.0827(9) 0.088(2) Uani 1 1 d . . .
H9A H 0.0810 0.7527 -0.0891 0.106 Uiso 1 1 calc R . .
C10 C 0.0503(7) 0.7061(3) 0.0436(7) 0.0751(19) Uani 1 1 d . . .
H10A H 0.1080 0.7208 0.1214 0.090 Uiso 1 1 calc R . .
C11 C 0.2886(5) 0.5126(2) 0.5814(5) 0.0544(14) Uani 1 1 d . . .
C12 C 0.3284(6) 0.4782(2) 0.5129(6) 0.0605(16) Uani 1 1 d . . .
H12A H 0.3550 0.4443 0.5391 0.073 Uiso 1 1 calc R . .
C13 C 0.3211(5) 0.5036(2) 0.3979(5) 0.0484(13) Uani 1 1 d . . .
C14 C 0.2802(7) 0.5064(3) 0.7158(6) 0.077(2) Uani 1 1 d . . .
H14A H 0.2502 0.5381 0.7369 0.115 Uiso 1 1 calc R . .
H14B H 0.3571 0.4992 0.7858 0.115 Uiso 1 1 calc R . .
H14C H 0.2281 0.4780 0.7100 0.115 Uiso 1 1 calc R . .
C15 C 0.3452(5) 0.4817(2) 0.2861(6) 0.0548(14) Uani 1 1 d . . .
C16 C 0.2891(9) 0.5014(3) 0.1541(7) 0.093(3) Uani 1 1 d . . .
H16A H 0.2366 0.5291 0.1366 0.111 Uiso 1 1 calc R . .
C17 C 0.3102(10) 0.4806(3) 0.0504(8) 0.110(3) Uani 1 1 d . . .
H17A H 0.2730 0.4944 -0.0365 0.132 Uiso 1 1 calc R . .
C18 C 0.3875(8) 0.4389(3) 0.0756(8) 0.088(2) Uani 1 1 d . . .
H18A H 0.4045 0.4252 0.0064 0.105 Uiso 1 1 calc R . .
C19 C 0.4370(7) 0.4187(3) 0.1998(8) 0.085(2) Uani 1 1 d . . .
H19A H 0.4864 0.3898 0.2157 0.102 Uiso 1 1 calc R . .
C20 C 0.4171(6) 0.4393(3) 0.3045(7) 0.0735(19) Uani 1 1 d . . .
H20A H 0.4531 0.4242 0.3900 0.088 Uiso 1 1 calc R . .
C21 C 0.3280(5) 0.6866(2) 0.6753(6) 0.0557(15) Uani 1 1 d . . .
C22 C 0.4166(6) 0.7165(2) 0.6682(6) 0.0585(15) Uani 1 1 d . . .
H22A H 0.4574 0.7434 0.7268 0.070 Uiso 1 1 calc R . .
C23 C 0.4337(5) 0.6988(2) 0.5557(5) 0.0498(13) Uani 1 1 d . . .
C24 C 0.2766(7) 0.6870(3) 0.7798(6) 0.078(2) Uani 1 1 d . . .
H24A H 0.2150 0.6613 0.7558 0.118 Uiso 1 1 calc R . .
H24B H 0.2449 0.7210 0.7822 0.118 Uiso 1 1 calc R . .
H24C H 0.3374 0.6789 0.8675 0.118 Uiso 1 1 calc R . .
C25 C 0.5254(5) 0.7146(2) 0.5120(5) 0.0506(13) Uani 1 1 d . . .
C26 C 0.5693(5) 0.6794(2) 0.4485(6) 0.0607(16) Uani 1 1 d . . .
H26A H 0.5395 0.6455 0.4312 0.073 Uiso 1 1 calc R . .
C27 C 0.6579(6) 0.6945(3) 0.4103(7) 0.078(2) Uani 1 1 d . . .
H27A H 0.6850 0.6710 0.3644 0.093 Uiso 1 1 calc R . .
C28 C 0.7055(7) 0.7432(4) 0.4390(8) 0.090(3) Uani 1 1 d . . .
H28A H 0.7666 0.7526 0.4157 0.108 Uiso 1 1 calc R . .
C29 C 0.6625(8) 0.7788(4) 0.5033(8) 0.092(3) Uani 1 1 d . . .
H29A H 0.6936 0.8124 0.5216 0.110 Uiso 1 1 calc R . .
C30 C 0.5736(6) 0.7644(3) 0.5403(6) 0.0718(18) Uani 1 1 d . . .
H30A H 0.5458 0.7882 0.5845 0.086 Uiso 1 1 calc R . .
C31 C 0.3167(6) 0.6404(3) 0.1507(6) 0.0678(18) Uani 1 1 d . . .
H31A H 0.2536 0.6270 0.0691 0.081 Uiso 1 1 calc R . .
H31B H 0.3176 0.6781 0.1417 0.081 Uiso 1 1 calc R . .
C32 C 0.4255(9) 0.6204(3) 0.1571(8) 0.081(2) Uani 1 1 d . . .
C33 C 0.075(2) 0.5606(11) -0.151(2) 0.254(10) Uiso 1 1 d U . .
C34 C -0.028(3) 0.5096(10) -0.199(3) 0.347(14) Uiso 1 1 d U . .
H34A H -0.0408 0.4985 -0.1223 0.520 Uiso 1 1 calc R . .
H34B H 0.0022 0.4808 -0.2324 0.520 Uiso 1 1 calc R . .
H34C H -0.1005 0.5215 -0.2693 0.520 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'
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'
Zn Zn 0.2839 1.4301 '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
C31 Zn1 N2 128.4(2) . . y
C31 Zn1 N3 124.4(2) . . y
N2 Zn1 N3 91.59(17) . . y
C31 Zn1 N1 119.2(2) . . y
N2 Zn1 N1 90.66(19) . . y
N3 Zn1 N1 92.85(18) . . y
C3 N1 N4 105.3(5) . . y
C3 N1 Zn1 138.2(4) . . y
N4 N1 Zn1 112.9(3) . . y
C13 N2 N5 106.6(4) . . y
C13 N2 Zn1 139.6(4) . . y
N5 N2 Zn1 111.2(3) . . y
C23 N3 N6 106.6(4) . . y
C23 N3 Zn1 138.8(4) . . y
N6 N3 Zn1 111.8(3) . . y
C1 N4 N1 110.5(5) . . y
C1 N4 B1 130.0(5) . . y
N1 N4 B1 119.3(4) . . y
C11 N5 N2 109.0(4) . . y
C11 N5 B1 130.5(5) . . y
N2 N5 B1 120.5(4) . . y
C21 N6 N3 109.7(5) . . y
C21 N6 B1 130.5(5) . . y
N3 N6 B1 119.7(4) . . y
N6 B1 N5 109.7(5) . . y
N6 B1 N4 109.2(5) . . y
N5 B1 N4 108.5(5) . . y
N4 C1 C2 106.8(5) . . y
N4 C1 C4 121.9(6) . . y
C2 C1 C4 131.3(6) . . y
C3 C2 C1 106.1(6) . . y
N1 C3 C2 111.3(5) . . y
N1 C3 C5 120.9(5) . . y
C2 C3 C5 127.9(6) . . y
C6 C5 C10 117.4(6) . . y
C6 C5 C3 121.9(6) . . y
C10 C5 C3 120.6(6) . . y
C5 C6 C7 121.0(7) . . y
C8 C7 C6 120.8(7) . . y
C7 C8 C9 119.6(7) . . y
C8 C9 C10 119.7(8) . . y
C9 C10 C5 121.4(7) . . y
N5 C11 C12 108.0(5) . . y
N5 C11 C14 122.1(5) . . y
C12 C11 C14 129.9(5) . . y
C11 C12 C13 106.7(5) . . y
N2 C13 C12 109.7(5) . . y
N2 C13 C15 122.7(5) . . y
C12 C13 C15 127.4(5) . . y
C20 C15 C16 116.8(6) . . y
C20 C15 C13 121.8(5) . . y
C16 C15 C13 121.2(6) . . y
C17 C16 C15 121.2(7) . . y
C16 C17 C18 119.7(7) . . y
C19 C18 C17 119.2(7) . . y
C18 C19 C20 121.6(7) . . y
C15 C20 C19 121.4(6) . . y
N6 C21 C22 107.7(5) . . y
N6 C21 C24 122.4(6) . . y
C22 C21 C24 129.8(5) . . y
C21 C22 C23 106.8(5) . . y
N3 C23 C22 109.1(5) . . y
N3 C23 C25 122.6(5) . . y
C22 C23 C25 128.1(5) . . y
C26 C25 C30 118.9(6) . . y
C26 C25 C23 120.6(5) . . y
C30 C25 C23 120.4(6) . . y
C25 C26 C27 120.1(6) . . y
C28 C27 C26 120.8(8) . . y
C27 C28 C29 119.6(7) . . y
C28 C29 C30 120.0(7) . . y
C29 C30 C25 120.6(7) . . y
C32 C31 Zn1 116.6(5) . . y
N7 C32 C31 178.5(10) . . y
N8 C33 C34 159(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
Zn1 C31 1.991(6) . y
Zn1 N2 2.069(4) . y
Zn1 N3 2.074(4) . y
Zn1 N1 2.072(5) . y
N1 C3 1.334(7) . y
N1 N4 1.371(6) . y
N2 C13 1.340(7) . y
N2 N5 1.384(6) . y
N3 C23 1.350(7) . y
N3 N6 1.383(6) . y
N4 C1 1.359(7) . y
N4 B1 1.557(8) . y
N5 C11 1.349(7) . y
N5 B1 1.544(8) . y
N6 C21 1.355(7) . y
N6 B1 1.526(8) . y
N7 C32 1.137(10) . y
N8 C33 1.22(5) . y
C1 C2 1.377(9) . y
C1 C4 1.505(9) . y
C2 C3 1.376(9) . y
C3 C5 1.496(8) . y
C5 C6 1.378(9) . y
C5 C10 1.381(9) . y
C6 C7 1.398(10) . y
C7 C8 1.340(11) . y
C8 C9 1.381(11) . y
C9 C10 1.392(10) . y
C11 C12 1.372(8) . y
C11 C14 1.515(7) . y
C12 C13 1.377(7) . y
C13 C15 1.478(7) . y
C15 C20 1.367(8) . y
C15 C16 1.401(8) . y
C16 C17 1.366(9) . y
C17 C18 1.388(11) . y
C18 C19 1.331(10) . y
C19 C20 1.368(9) . y
C21 C22 1.374(9) . y
C21 C24 1.520(8) . y
C22 C23 1.399(8) . y
C23 C25 1.468(8) . y
C25 C26 1.379(8) . y
C25 C30 1.386(8) . y
C26 C27 1.390(9) . y
C27 C28 1.358(11) . y
C28 C29 1.385(11) . y
C29 C30 1.379(10) . y
C31 C32 1.426(11) . y
C33 C34 1.75(3) . y
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2024-11-15T14:40:08+02:00
;
 Removed multiple data items that had the 'Y' placeholder value.
;
