#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:33:58 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178625 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/36/4073668.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_4073668
loop_
_publ_author_name
'Zenkina, Olena'
'Altman, Marc'
'Leitus, Gregory'
'Shimon, Linda J. W.'
'Cohen, Revital'
'van der Boom, Milko E.'
_publ_section_title
;
 From Azobenzene Coordination to Aryl−Halide Bond Activation by
 Platinum
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4528
_journal_paper_doi               10.1021/om700519v
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C23 H39 N3 P2 Pt'
_chemical_formula_weight         614.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.851(4)
_cell_length_b                   7.9190(16)
_cell_length_c                   8.3420(17)
_cell_measurement_reflns_used    12892
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1245.3(4)
_computing_cell_refinement       HKL
_computing_data_collection       'Collect package (Bruker Nonius)'
_computing_data_reduction        HKL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1604
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    5.777
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.161
_refine_diff_density_min         -1.674
_refine_diff_density_rms         0.161
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.506(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         1604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0300
_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)+(0.0421P)²+4.8564P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0749
_reflns_number_gt                1492
_reflns_number_total             1604
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700519v-file004.cif
_cod_data_source_block           v21aa
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2
_cod_database_code               4073668
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_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
Pt1 Pt 0.5000 0.5000 0.52673(4) 0.01432(12) Uani 1 2 d S . .
P1 P 0.42480(10) 0.6211(2) 0.3513(2) 0.0131(4) Uani 1 1 d . . .
N1 N 0.4693(4) 0.5529(8) 0.7635(7) 0.0159(13) Uani 1 1 d . . .
C1 C 0.4078(4) 0.4592(8) 0.8020(10) 0.0173(16) Uani 1 1 d . . .
C2 C 0.4058(4) 0.2862(9) 0.8315(9) 0.0149(15) Uani 1 1 d . C .
H2 H 0.4469 0.2215 0.8250 0.018 Uiso 1 1 calc R . .
C3 C 0.3444(4) 0.5501(9) 0.8130(8) 0.0137(15) Uani 1 1 d . C .
H3 H 0.3445 0.6659 0.7946 0.016 Uiso 1 1 calc R . .
C4 C 0.3416(4) 0.2125(10) 0.8706(9) 0.0189(16) Uani 1 1 d . . .
H4 H 0.3409 0.0970 0.8906 0.023 Uiso 1 1 calc R A 1
C5 C 0.2820(4) 0.4696(11) 0.8506(9) 0.021(2) Uani 1 1 d . . .
H5 H 0.2404 0.5324 0.8554 0.026 Uiso 1 1 calc R B 1
C6 C 0.2791(4) 0.2989(9) 0.8816(9) 0.0213(16) Uani 0.50 1 d P C 1
H6 H 0.2369 0.2453 0.9085 0.026 Uiso 0.50 1 calc PR C 1
N6 N 0.2791(4) 0.2989(9) 0.8816(9) 0.0213(16) Uani 0.50 1 d P C 2
C7 C 0.3620(4) 0.4781(13) 0.2530(10) 0.0221(19) Uani 1 1 d . . .
H7A H 0.3277 0.5443 0.1935 0.026 Uiso 1 1 calc R . .
H7B H 0.3875 0.4078 0.1771 0.026 Uiso 1 1 calc R . .
C8 C 0.4662(5) 0.7352(10) 0.1853(10) 0.0214(17) Uani 1 1 d . . .
H8A H 0.5062 0.7979 0.2274 0.026 Uiso 1 1 calc R . .
H8B H 0.4847 0.6528 0.1101 0.026 Uiso 1 1 calc R . .
C9 C 0.3657(4) 0.7749(9) 0.4445(10) 0.0178(16) Uani 1 1 d . . .
H9A H 0.3361 0.8250 0.3622 0.021 Uiso 1 1 calc R . .
H9B H 0.3349 0.7167 0.5194 0.021 Uiso 1 1 calc R . .
C10 C 0.3229(6) 0.3651(12) 0.3716(12) 0.037(2) Uani 1 1 d . . .
H10A H 0.3566 0.2972 0.4291 0.056 Uiso 1 1 calc R . .
H10B H 0.2906 0.2931 0.3146 0.056 Uiso 1 1 calc R . .
H10C H 0.2969 0.4339 0.4459 0.056 Uiso 1 1 calc R . .
C11 C 0.4188(4) 0.8580(9) 0.0927(10) 0.0215(16) Uani 1 1 d . . .
H11A H 0.3771 0.8000 0.0563 0.032 Uiso 1 1 calc R . .
H11B H 0.4443 0.9015 0.0020 0.032 Uiso 1 1 calc R . .
H11C H 0.4053 0.9496 0.1616 0.032 Uiso 1 1 calc R . .
C12 C 0.4053(5) 0.9171(10) 0.5343(10) 0.0253(18) Uani 1 1 d . . .
H12A H 0.4359 0.8685 0.6139 0.038 Uiso 1 1 calc R . .
H12B H 0.3715 0.9901 0.5853 0.038 Uiso 1 1 calc R . .
H12C H 0.4331 0.9811 0.4595 0.038 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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 Pt1 N1 39.8(3) . 2_665
N1 Pt1 P1 150.42(18) . 2_665
N1 Pt1 P1 110.64(17) 2_665 2_665
N1 Pt1 P1 110.64(17) . .
N1 Pt1 P1 150.42(18) 2_665 .
P1 Pt1 P1 98.93(10) 2_665 .
C9 P1 C8 104.7(4) . .
C9 P1 C7 102.1(4) . .
C8 P1 C7 104.0(4) . .
C9 P1 Pt1 113.1(3) . .
C8 P1 Pt1 115.7(3) . .
C7 P1 Pt1 115.8(3) . .
C1 N1 N1 110.9(7) . 2_665
C1 N1 Pt1 109.6(5) . .
N1 N1 Pt1 70.10(17) 2_665 .
C2 C1 C3 118.1(7) . .
C2 C1 N1 125.4(7) . .
C3 C1 N1 116.5(6) . .
C4 C2 C1 118.7(7) . .
C4 C2 H2 120.6 . .
C1 C2 H2 120.6 . .
C5 C3 C1 120.5(7) . .
C5 C3 H3 119.7 . .
C1 C3 H3 119.7 . .
C6 C4 C2 124.0(7) . .
C6 C4 H4 118.0 . .
C2 C4 H4 118.0 . .
C3 C5 C6 122.1(7) . .
C3 C5 H5 118.9 . .
C6 C5 H5 118.9 . .
C4 C6 C5 116.5(7) . .
C4 C6 H6 121.8 . .
C5 C6 H6 121.8 . .
C10 C7 P1 112.6(6) . .
C10 C7 H7A 109.1 . .
P1 C7 H7A 109.1 . .
C10 C7 H7B 109.1 . .
P1 C7 H7B 109.1 . .
H7A C7 H7B 107.8 . .
C11 C8 P1 116.6(6) . .
C11 C8 H8A 108.1 . .
P1 C8 H8A 108.1 . .
C11 C8 H8B 108.1 . .
P1 C8 H8B 108.1 . .
H8A C8 H8B 107.3 . .
C12 C9 P1 113.5(6) . .
C12 C9 H9A 108.9 . .
P1 C9 H9A 108.9 . .
C12 C9 H9B 108.9 . .
P1 C9 H9B 108.9 . .
H9A C9 H9B 107.7 . .
C7 C10 H10A 109.5 . .
C7 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C7 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C8 C11 H11A 109.5 . .
C8 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C8 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C9 C12 H12A 109.5 . .
C9 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C9 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 N1 2.100(6) .
Pt1 N1 2.101(6) 2_665
Pt1 P1 2.2516(19) 2_665
Pt1 P1 2.2516(19) .
P1 C9 1.824(8) .
P1 C8 1.828(8) .
P1 C7 1.831(9) .
N1 C1 1.412(10) .
N1 N1 1.430(13) 2_665
C1 C2 1.392(10) .
C1 C3 1.399(10) .
C2 C4 1.384(11) .
C2 H2 0.9300 .
C3 C5 1.375(11) .
C3 H3 0.9300 .
C4 C6 1.365(11) .
C4 H4 0.9300 .
C5 C6 1.377(10) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 C10 1.524(12) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C11 1.530(11) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C12 1.545(11) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 Pt1 P1 C9 12.6(3) . .
N1 Pt1 P1 C9 14.5(5) 2_665 .
P1 Pt1 P1 C9 -166.7(3) 2_665 .
N1 Pt1 P1 C8 133.3(4) . .
N1 Pt1 P1 C8 135.2(5) 2_665 .
P1 Pt1 P1 C8 -46.0(3) 2_665 .
N1 Pt1 P1 C7 -104.6(4) . .
N1 Pt1 P1 C7 -102.7(5) 2_665 .
P1 Pt1 P1 C7 76.0(3) 2_665 .
N1 Pt1 N1 C1 -105.9(7) 2_665 .
P1 Pt1 N1 C1 -108.6(5) 2_665 .
P1 Pt1 N1 C1 72.7(5) . .
P1 Pt1 N1 N1 -2.7(8) 2_665 2_665
P1 Pt1 N1 N1 178.6(4) . 2_665
N1 N1 C1 C2 -1.9(9) 2_665 .
Pt1 N1 C1 C2 73.6(9) . .
N1 N1 C1 C3 177.2(6) 2_665 .
Pt1 N1 C1 C3 -107.3(7) . .
C3 C1 C2 C4 -0.2(12) . .
N1 C1 C2 C4 178.9(7) . .
C2 C1 C3 C5 -0.5(12) . .
N1 C1 C3 C5 -179.7(7) . .
C1 C2 C4 C6 0.3(13) . .
C1 C3 C5 C6 1.1(12) . .
C2 C4 C6 C5 0.2(13) . .
C3 C5 C6 C4 -0.9(12) . .
C9 P1 C7 C10 -73.2(8) . .
C8 P1 C7 C10 178.1(7) . .
Pt1 P1 C7 C10 50.0(8) . .
C9 P1 C8 C11 -38.3(7) . .
C7 P1 C8 C11 68.5(7) . .
Pt1 P1 C8 C11 -163.4(5) . .
C8 P1 C9 C12 -70.3(7) . .
C7 P1 C9 C12 -178.4(6) . .
Pt1 P1 C9 C12 56.6(6) . .
