#------------------------------------------------------------------------------
#$Date: 2024-11-15 14:46:36 +0200 (Fri, 15 Nov 2024) $
#$Revision: 295934 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/15/4311577.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_4311577
loop_
_publ_author_name
'Horst Brombacher'
'Heinrich Vahrenkamp'
_publ_section_title
;
 Pyrazolylborate-Zinc Alkoxide Complexes. 1. Basic Properties,
 Methylations, and Heterocumulene Insertions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6042
_journal_page_last               6049
_journal_paper_doi               10.1021/ic049179v
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C31 H31 B N6 O Zn'
_chemical_formula_weight         579.80
_chemical_melting_point          229
_chemical_name_common            Tp(Ph,Me)Zn-OMe
_chemical_name_systematic
; 
 Hydrotris(3-phenyl-5-methylpyrazol-1-yl)borato-zink-methanolat 
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.140(4)
_cell_angle_beta                 102.985(4)
_cell_angle_gamma                90.631(4)
_cell_formula_units_Z            2
_cell_length_a                   9.0614(19)
_cell_length_b                   9.912(2)
_cell_length_c                   16.412(3)
_cell_measurement_temperature    248(2)
_cell_volume                     1375.5(5)
_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      248(2)
_diffrn_measured_fraction_theta_full 0.887
_diffrn_measured_fraction_theta_max 0.887
_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  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12361
_diffrn_reflns_theta_full        28.83
_diffrn_reflns_theta_max         28.83
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       isometric
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0735P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1422
_reflns_number_gt                4076
_reflns_number_total             6385
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049179vsi20040706_092342_1.cif
_cod_data_source_block           horjm
_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 2.4.1 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 (73
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 (47 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1375.4(5)
_cod_database_code               4311577
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.68945(4) 0.90716(4) 0.74144(2) 0.03504(14) Uani 1 1 d . . .
N1 N 0.6335(3) 1.0999(3) 0.71989(16) 0.0325(6) Uani 1 1 d . . .
N2 N 0.7103(3) 0.9883(3) 0.87378(17) 0.0329(6) Uani 1 1 d . . .
N3 N 0.9222(3) 0.9390(3) 0.75592(17) 0.0341(6) Uani 1 1 d . . .
N4 N 0.7243(3) 1.2082(3) 0.78331(17) 0.0347(6) Uani 1 1 d . . .
N5 N 0.8189(3) 1.1024(3) 0.90639(16) 0.0332(6) Uani 1 1 d . . .
N6 N 0.9649(3) 1.0804(3) 0.79027(17) 0.0331(6) Uani 1 1 d . . .
O1 O 0.5790(3) 0.7369(3) 0.68356(16) 0.0513(7) Uani 1 1 d . . .
B1 B 0.8671(4) 1.1760(4) 0.8445(2) 0.0357(8) Uani 1 1 d . . .
H1 H 0.9275 1.2655 0.8794 0.043 Uiso 1 1 calc R . .
C1 C 0.6712(4) 1.3326(3) 0.7785(2) 0.0390(8) Uani 1 1 d . . .
C2 C 0.5442(4) 1.3063(4) 0.7111(2) 0.0431(8) Uani 1 1 d . . .
H2A H 0.4833 1.3733 0.6924 0.052 Uiso 1 1 calc R . .
C3 C 0.5232(4) 1.1601(3) 0.6755(2) 0.0353(7) Uani 1 1 d . . .
C4 C 0.7435(4) 1.4710(4) 0.8397(3) 0.0534(10) Uani 1 1 d . . .
H4A H 0.8328 1.4554 0.8803 0.080 Uiso 1 1 calc R . .
H4B H 0.6716 1.5177 0.8718 0.080 Uiso 1 1 calc R . .
H4C H 0.7728 1.5297 0.8066 0.080 Uiso 1 1 calc R . .
C5 C 0.4048(4) 1.0800(4) 0.5990(2) 0.0375(8) Uani 1 1 d . . .
C6 C 0.2991(5) 1.1518(5) 0.5562(3) 0.0607(11) Uani 1 1 d . . .
H6A H 0.3026 1.2505 0.5775 0.073 Uiso 1 1 calc R . .
C7 C 0.1884(5) 1.0823(6) 0.4829(3) 0.0737(14) Uani 1 1 d . . .
H7A H 0.1181 1.1339 0.4550 0.088 Uiso 1 1 calc R . .
C8 C 0.1807(4) 0.9388(5) 0.4507(3) 0.0591(11) Uani 1 1 d . . .
H8A H 0.1056 0.8912 0.4009 0.071 Uiso 1 1 calc R . .
C9 C 0.2838(5) 0.8657(5) 0.4921(3) 0.0615(11) Uani 1 1 d . . .
H9A H 0.2797 0.7671 0.4703 0.074 Uiso 1 1 calc R . .
C10 C 0.3943(4) 0.9351(4) 0.5659(2) 0.0503(9) Uani 1 1 d . . .
H10A H 0.4634 0.8827 0.5939 0.060 Uiso 1 1 calc R . .
C11 C 0.8621(4) 1.1322(3) 0.9938(2) 0.0348(7) Uani 1 1 d . . .
C12 C 0.7820(4) 1.0390(3) 1.0194(2) 0.0376(8) Uani 1 1 d . . .
H12A H 0.7893 1.0350 1.0767 0.045 Uiso 1 1 calc R . .
C13 C 0.6877(3) 0.9518(3) 0.9431(2) 0.0310(7) Uani 1 1 d . . .
C14 C 0.9782(4) 1.2494(4) 1.0497(2) 0.0464(9) Uani 1 1 d . . .
H14A H 1.0143 1.2976 1.0131 0.070 Uiso 1 1 calc R . .
H14B H 1.0628 1.2110 1.0814 0.070 Uiso 1 1 calc R . .
H14C H 0.9326 1.3155 1.0908 0.070 Uiso 1 1 calc R . .
C15 C 0.5768(3) 0.8360(3) 0.9364(2) 0.0328(7) Uani 1 1 d . . .
C16 C 0.4781(4) 0.7615(4) 0.8581(2) 0.0430(8) Uani 1 1 d . . .
H16A H 0.4786 0.7854 0.8066 0.052 Uiso 1 1 calc R . .
C17 C 0.3789(4) 0.6520(4) 0.8557(3) 0.0515(10) Uani 1 1 d . . .
H17A H 0.3135 0.6014 0.8025 0.062 Uiso 1 1 calc R . .
C18 C 0.3756(4) 0.6167(4) 0.9310(3) 0.0509(10) Uani 1 1 d . . .
H18A H 0.3090 0.5418 0.9289 0.061 Uiso 1 1 calc R . .
C19 C 0.4702(4) 0.6918(4) 1.0089(3) 0.0524(10) Uani 1 1 d . . .
H19A H 0.4677 0.6688 1.0604 0.063 Uiso 1 1 calc R . .
C20 C 0.5692(4) 0.8012(4) 1.0115(2) 0.0434(8) Uani 1 1 d . . .
H20A H 0.6324 0.8527 1.0653 0.052 Uiso 1 1 calc R . .
C21 C 1.1018(3) 1.1087(4) 0.7762(2) 0.0367(7) Uani 1 1 d . . .
C22 C 1.1499(4) 0.9834(4) 0.7336(2) 0.0411(8) Uani 1 1 d . . .
H22A H 1.2414 0.9704 0.7156 0.049 Uiso 1 1 calc R . .
C23 C 1.0363(4) 0.8792(3) 0.7223(2) 0.0354(7) Uani 1 1 d . . .
C24 C 1.1760(4) 1.2547(4) 0.8027(3) 0.0498(9) Uani 1 1 d . . .
H24A H 1.1119 1.3207 0.8310 0.075 Uiso 1 1 calc R . .
H24B H 1.1905 1.2785 0.7513 0.075 Uiso 1 1 calc R . .
H24C H 1.2738 1.2599 0.8429 0.075 Uiso 1 1 calc R . .
C25 C 1.0361(4) 0.7256(3) 0.6838(2) 0.0369(7) Uani 1 1 d . . .
C26 C 1.1402(4) 0.6725(4) 0.6349(3) 0.0516(9) Uani 1 1 d . . .
H26A H 1.2095 0.7347 0.6257 0.062 Uiso 1 1 calc R . .
C27 C 1.1430(5) 0.5296(4) 0.5998(3) 0.0622(11) Uani 1 1 d . . .
H27A H 1.2135 0.4953 0.5663 0.075 Uiso 1 1 calc R . .
C28 C 1.0439(5) 0.4367(4) 0.6130(3) 0.0539(10) Uani 1 1 d . . .
H28A H 1.0467 0.3391 0.5890 0.065 Uiso 1 1 calc R . .
C29 C 0.9415(4) 0.4870(4) 0.6612(2) 0.0491(9) Uani 1 1 d . . .
H29A H 0.8732 0.4235 0.6702 0.059 Uiso 1 1 calc R . .
C30 C 0.9369(4) 0.6306(4) 0.6971(2) 0.0428(8) Uani 1 1 d . . .
H30A H 0.8662 0.6638 0.7307 0.051 Uiso 1 1 calc R . .
C31 C 0.5753(5) 0.6434(5) 0.6018(3) 0.0700(13) Uani 1 1 d . . .
H31A H 0.5049 0.5625 0.5914 0.105 Uiso 1 1 calc R . .
H31B H 0.6760 0.6123 0.6002 0.105 Uiso 1 1 calc R . .
H31C H 0.5422 0.6903 0.5570 0.105 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'
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'
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
O1 Zn1 N2 118.96(11) . . y
O1 Zn1 N3 123.74(11) . . y
N2 Zn1 N3 91.78(10) . . y
O1 Zn1 N1 125.26(11) . . y
N2 Zn1 N1 91.85(10) . . y
N3 Zn1 N1 96.53(10) . . y
C3 N1 N4 106.3(2) . . y
C3 N1 Zn1 142.0(2) . . y
N4 N1 Zn1 110.23(18) . . y
C13 N2 N5 106.4(2) . . y
C13 N2 Zn1 141.4(2) . . y
N5 N2 Zn1 109.20(18) . . y
C23 N3 N6 106.7(2) . . y
C23 N3 Zn1 140.7(2) . . y
N6 N3 Zn1 109.01(18) . . y
C1 N4 N1 110.1(3) . . y
C1 N4 B1 129.9(3) . . y
N1 N4 B1 120.0(2) . . y
C11 N5 N2 109.4(2) . . y
C11 N5 B1 130.2(3) . . y
N2 N5 B1 120.4(2) . . y
C21 N6 N3 109.9(3) . . y
C21 N6 B1 130.4(3) . . y
N3 N6 B1 119.3(2) . . y
C31 O1 Zn1 130.7(3) . . y
N5 B1 N6 109.7(3) . . y
N5 B1 N4 109.6(3) . . y
N6 B1 N4 110.0(3) . . y
N4 C1 C2 107.9(3) . . y
N4 C1 C4 123.2(3) . . y
C2 C1 C4 128.8(3) . . y
C1 C2 C3 106.3(3) . . y
N1 C3 C2 109.4(3) . . y
N1 C3 C5 123.7(3) . . y
C2 C3 C5 126.9(3) . . y
C6 C5 C10 117.1(3) . . y
C6 C5 C3 119.3(3) . . y
C10 C5 C3 123.6(3) . . y
C5 C6 C7 121.7(4) . . y
C8 C7 C6 120.3(4) . . y
C9 C8 C7 119.0(4) . . y
C8 C9 C10 120.8(4) . . y
C5 C10 C9 121.1(4) . . y
N5 C11 C12 108.3(3) . . y
N5 C11 C14 123.3(3) . . y
C12 C11 C14 128.4(3) . . y
C11 C12 C13 106.1(3) . . y
N2 C13 C12 109.8(3) . . y
N2 C13 C15 123.4(3) . . y
C12 C13 C15 126.8(3) . . y
C20 C15 C16 118.3(3) . . y
C20 C15 C13 118.7(3) . . y
C16 C15 C13 123.0(3) . . y
C17 C16 C15 120.3(3) . . y
C18 C17 C16 120.5(4) . . y
C19 C18 C17 119.6(3) . . y
C18 C19 C20 120.1(4) . . y
C19 C20 C15 121.2(3) . . y
N6 C21 C22 107.6(3) . . y
N6 C21 C24 122.6(3) . . y
C22 C21 C24 129.8(3) . . y
C21 C22 C23 106.6(3) . . y
N3 C23 C22 109.2(3) . . y
N3 C23 C25 122.8(3) . . y
C22 C23 C25 128.0(3) . . y
C26 C25 C30 118.2(3) . . y
C26 C25 C23 120.0(3) . . y
C30 C25 C23 121.8(3) . . y
C27 C26 C25 120.6(4) . . y
C28 C27 C26 120.7(4) . . y
C29 C28 C27 119.4(4) . . y
C28 C29 C30 120.7(4) . . y
C29 C30 C25 120.3(3) . . 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 O1 1.843(2) . y
Zn1 N2 2.059(3) . y
Zn1 N3 2.079(3) . y
Zn1 N1 2.085(3) . y
N1 C3 1.346(4) . y
N1 N4 1.374(3) . y
N2 C13 1.341(4) . y
N2 N5 1.391(3) . y
N3 C23 1.346(4) . y
N3 N6 1.372(3) . y
N4 C1 1.345(4) . y
N4 B1 1.545(4) . y
N5 C11 1.345(4) . y
N5 B1 1.535(5) . y
N6 C21 1.353(4) . y
N6 B1 1.543(5) . y
O1 C31 1.395(5) . y
C1 C2 1.370(5) . y
C1 C4 1.496(5) . y
C2 C3 1.397(5) . y
C3 C5 1.477(4) . y
C5 C6 1.381(5) . y
C5 C10 1.381(5) . y
C6 C7 1.382(6) . y
C7 C8 1.368(6) . y
C8 C9 1.364(6) . y
C9 C10 1.385(5) . y
C11 C12 1.377(5) . y
C11 C14 1.498(4) . y
C12 C13 1.396(4) . y
C13 C15 1.480(4) . y
C15 C20 1.386(5) . y
C15 C16 1.392(5) . y
C16 C17 1.388(5) . y
C17 C18 1.380(5) . y
C18 C19 1.374(6) . y
C19 C20 1.384(5) . y
C21 C22 1.373(5) . y
C21 C24 1.495(4) . y
C22 C23 1.394(4) . y
C23 C25 1.477(5) . y
C25 C26 1.388(5) . y
C25 C30 1.389(5) . y
C26 C27 1.375(5) . y
C27 C28 1.372(5) . y
C28 C29 1.363(5) . y
C29 C30 1.386(5) . 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.
;
