#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/75/4077555.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_4077555
loop_
_publ_author_name
'Reinartz, Stefan'
'White, Peter S.'
'Brookhart, Maurice'
'Templeton, Joseph L.'
_publ_section_title
;
 Acid-Assisted Reductive Elimination as a Route to Platinum(II) Products
 from Platinum(IV) Tris(pyrazolyl)borate Reagents
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              3854
_journal_paper_doi               10.1021/om000440z
_journal_volume                  19
_journal_year                    2000
_chemical_formula_moiety         'Pt S C18 H31 B N6 '
_chemical_formula_sum            'C18 H31 B N6 Pt S'
_chemical_formula_weight         569.44
_chemical_name_systematic        ?
_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'
_cell_angle_alpha                90.0
_cell_angle_beta                 111.752(1)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   16.2303(4)
_cell_length_b                   8.50990(20)
_cell_length_c                   17.1741(4)
_cell_measurement_reflns_used    7643
_cell_measurement_temperature    193
_cell_measurement_theta_max      35.00
_cell_measurement_theta_min      2.50
_cell_volume                     2203.16(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT/NRCVAX DATRD2'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    'NRCVAX SOLVER'
_diffrn_ambient_temperature      193
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_method       'Omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            88726
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         0.00
_exptl_absorpt_coefficient_mu    6.45
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_F_000             1115.92
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.54
_refine_diff_density_min         -1.81
_refine_ls_extinction_coef       3.782(253)
_refine_ls_extinction_method     Larson
_refine_ls_goodness_of_fit_obs   1.96
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         8895
_refine_ls_R_factor_all          0.032
_refine_ls_R_factor_obs          0.028
_refine_ls_shift/esd_max         0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/(σ²(F)+0.0002F²)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.042
_refine_ls_wR_factor_obs         0.041
_reflns_number_observed          8897
_reflns_number_total             9735
_reflns_observed_criterion       'Inet > 2.5\s(Inet)'
_cod_data_source_file            om000440z.cif
_cod_data_source_block           c00029
_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 2.4.2 from 2011-04-26.

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 '1/(\s^2^(F)+0.0002F^2^)' 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^(F)+0.0002F^2^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'Pt S C18 H31 B N6 '
_cod_database_code               4077555
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,1/2+y,1/2-z
x,1/2-y,1/2+z
loop_
_atom_site_label
_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_type_symbol
Pt1 0.747985(6) 0.479667(12) 0.090064(5) 0.01652(5) Uij Pt
S1 0.70380(5) 0.67115(9) -0.00695(4) 0.0277(3) Uij S
C1 0.64465(21) 0.3374(4) 0.02169(19) 0.0311(14) Uij C
C2 0.6941(3) 0.6017(5) -0.10774(21) 0.0446(21) Uij C
C3 0.5880(3) 0.7101(6) -0.0297(3) 0.058(3) Uij C
B10 0.79756(20) 0.5578(4) 0.28253(18) 0.0188(12) Uij B
N11 0.78770(14) 0.3239(3) 0.18717(13) 0.0186(10) Uij N
N12 0.79988(14) 0.3802(3) 0.26601(13) 0.0188(10) Uij N
C13 0.81873(17) 0.2567(3) 0.31895(16) 0.0220(12) Uij C
C14 0.81943(20) 0.1222(3) 0.27588(19) 0.0266(14) Uij C
C15 0.80016(18) 0.1681(3) 0.19270(17) 0.0225(12) Uij C
C16 0.83364(22) 0.2742(4) 0.41068(18) 0.0318(16) Uij C
C17 0.80089(25) 0.0695(4) 0.12152(22) 0.0338(17) Uij C
N21 0.85358(14) 0.6217(3) 0.16731(13) 0.0183(9) Uij N
N22 0.86335(14) 0.6400(3) 0.24953(13) 0.0183(9) Uij N
C23 0.93598(17) 0.7278(3) 0.28919(16) 0.0218(11) Uij C
C24 0.97324(19) 0.7683(4) 0.23115(18) 0.0257(13) Uij C
C25 0.92011(17) 0.6994(3) 0.15627(17) 0.0225(12) Uij C
C26 0.96777(21) 0.7648(4) 0.38092(19) 0.0338(15) Uij C
C27 0.93012(22) 0.7026(4) 0.07358(20) 0.0336(17) Uij C
N31 0.69308(15) 0.7774(3) 0.20945(15) 0.0221(10) Uij N
N32 0.70288(14) 0.62408(25) 0.23648(13) 0.0179(9) Uij N
C33 0.62275(18) 0.5601(3) 0.22558(18) 0.0220(12) Uij C
C34 0.55923(18) 0.6730(3) 0.18996(17) 0.0240(12) Uij C
C35 0.60683(19) 0.8060(3) 0.18173(17) 0.0241(12) Uij C
C36 0.60884(21) 0.3950(4) 0.24898(25) 0.0355(17) Uij C
C37 0.5712(3) 0.9652(4) 0.1475(3) 0.0396(19) Uij C
H1a 0.612 0.386 -0.031 0.0392 Uiso H
H1b 0.667 0.238 0.012 0.0392 Uiso H
H1c 0.606 0.322 0.052 0.0392 Uiso H
H2a 0.752 0.575 -0.107 0.0560 Uiso H
H2b 0.657 0.511 -0.122 0.0560 Uiso H
H2c 0.669 0.682 -0.149 0.0560 Uiso H
H3a 0.580 0.750 0.020 0.0687 Uiso H
H3b 0.567 0.786 -0.074 0.0687 Uiso H
H3c 0.555 0.614 -0.047 0.0687 Uiso H
H10 0.815 0.576 0.342 0.0291 Uiso H
H14 0.830 0.017 0.298 0.0369 Uiso H
H16a 0.846 0.174 0.438 0.0419 Uiso H
H16b 0.883 0.343 0.437 0.0419 Uiso H
H16c 0.781 0.318 0.416 0.0419 Uiso H
H17a 0.811 -0.038 0.139 0.0445 Uiso H
H17b 0.745 0.078 0.076 0.0445 Uiso H
H17c 0.847 0.104 0.103 0.0445 Uiso H
H24 1.025 0.831 0.241 0.0355 Uiso H
H26a 1.020 0.828 0.396 0.0413 Uiso H
H26b 0.922 0.821 0.393 0.0413 Uiso H
H26c 0.981 0.669 0.413 0.0413 Uiso H
H27a 0.981 0.764 0.078 0.0458 Uiso H
H27b 0.937 0.597 0.057 0.0458 Uiso H
H27c 0.878 0.749 0.032 0.0458 Uiso H
H34 0.496 0.663 0.175 0.0340 Uiso H
H36a 0.547 0.377 0.236 0.0463 Uiso H
H36b 0.630 0.323 0.218 0.0463 Uiso H
H36c 0.640 0.379 0.308 0.0463 Uiso H
H37a 0.508 0.965 0.130 0.0504 Uiso H
H37b 0.596 1.044 0.190 0.0504 Uiso H
H37c 0.587 0.989 0.100 0.0504 Uiso H
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pt -1.703 8.391 'International Tables Vol. IV Table 2.2B'
S 0.125 0.123 'International Tables Vol. IV Table 2.2B'
C 0.003 0.002 'International Tables Vol. IV Table 2.2B'
H 0.000 0.000 'International Tables Vol. IV Table 2.2B'
B 0.001 0.001 'International Tables Vol. IV Table 2.2B'
N 0.006 0.003 'International Tables Vol. IV Table 2.2B'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
S(1) Pt(1) C(1) 92.00(9)
S(1) Pt(1) N(11) 173.82(6)
S(1) Pt(1) N(21) 90.72(6)
C(1) Pt(1) N(11) 91.61(11)
C(1) Pt(1) N(21) 176.51(11)
N(11) Pt(1) N(21) 85.49(8)
Pt(1) S(1) C(2) 111.64(14)
Pt(1) S(1) C(3) 108.31(15)
C(2) S(1) C(3) 98.13(21)
N(12) B(10) N(22) 107.96(21)
N(12) B(10) N(32) 110.49(21)
N(22) B(10) N(32) 109.66(21)
Pt(1) N(11) N(12) 117.63(16)
Pt(1) N(11) C(15) 134.05(18)
N(12) N(11) C(15) 108.14(20)
B(10) N(12) N(11) 121.12(20)
B(10) N(12) C(13) 130.93(22)
N(11) N(12) C(13) 107.78(22)
N(12) C(13) C(14) 109.48(23)
N(12) C(13) C(16) 122.4(3)
C(14) C(13) C(16) 128.2(3)
C(13) C(14) C(15) 105.98(24)
N(11) C(15) C(14) 108.62(24)
N(11) C(15) C(17) 123.19(25)
C(14) C(15) C(17) 128.0(3)
Pt(1) N(21) N(22) 117.97(15)
Pt(1) N(21) C(25) 134.62(18)
N(22) N(21) C(25) 107.36(21)
B(10) N(22) N(21) 119.57(20)
B(10) N(22) C(23) 131.13(22)
N(21) N(22) C(23) 109.24(21)
N(22) C(23) C(24) 107.89(23)
N(22) C(23) C(26) 122.95(25)
C(24) C(23) C(26) 129.1(3)
C(23) C(24) C(25) 105.93(23)
N(21) C(25) C(24) 109.58(23)
N(21) C(25) C(27) 121.6(3)
C(24) C(25) C(27) 128.9(3)
N(32) N(31) C(35) 105.70(22)
B(10) N(32) N(31) 119.10(21)
B(10) N(32) C(33) 129.98(22)
N(31) N(32) C(33) 110.43(21)
N(32) C(33) C(34) 107.67(24)
N(32) C(33) C(36) 124.7(3)
C(34) C(33) C(36) 127.6(3)
C(33) C(34) C(35) 104.93(24)
N(31) C(35) C(34) 111.27(24)
N(31) C(35) C(37) 120.5(3)
C(34) C(35) C(37) 128.2(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pt(1) S(1) 2.2495(7)
Pt(1) C(1) 2.049(3)
Pt(1) N(11) 2.0392(21)
Pt(1) N(21) 2.1147(21)
S(1) C(2) 1.780(4)
S(1) C(3) 1.803(4)
B(10) N(12) 1.541(4)
B(10) N(22) 1.549(4)
B(10) N(32) 1.551(4)
N(11) N(12) 1.380(3)
N(11) C(15) 1.339(3)
N(12) C(13) 1.348(3)
C(13) C(14) 1.365(4)
C(13) C(16) 1.510(4)
C(14) C(15) 1.400(4)
C(15) C(17) 1.486(4)
N(21) N(22) 1.370(3)
N(21) C(25) 1.338(3)
N(22) C(23) 1.348(3)
C(23) C(24) 1.387(4)
C(23) C(26) 1.498(4)
C(24) C(25) 1.386(4)
C(25) C(27) 1.488(4)
N(31) N(32) 1.375(3)
N(31) C(35) 1.324(4)
N(32) C(33) 1.357(3)
C(33) C(34) 1.375(4)
C(33) C(36) 1.502(4)
C(34) C(35) 1.407(4)
C(35) C(37) 1.504(4)
