#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:59:02 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180021 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/15/7031510.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_7031510
loop_
_publ_author_name
'Scheuermann, Margaret L.'
'Grice, Kyle A.'
'Ruppel, Matthew J.'
'Roselló-Merino, Marta'
'Kaminsky, Werner'
'Goldberg, Karen I.'
_publ_section_title
;
 Hemilability of P(X)N-type ligands (X = O, N-H): rollover cyclometalation
 and benzene C-H activation from (P(X)N)PtMe2 complexes.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12018
_journal_page_last               12025
_journal_paper_doi               10.1039/c4dt01143k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C15 H29 N2 P Pt'
_chemical_formula_sum            'C15 H29 N2 P Pt'
_chemical_formula_weight         463.46
_chemical_name_common            (tBuP(N-H)N)PtMe2
_chemical_name_systematic
;
 (tBuP(N-H)N)PtMe2
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2014-04-09T10:47:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.8300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4311(4)
_cell_length_b                   8.6437(2)
_cell_length_c                   13.5536(3)
_cell_measurement_reflns_used    1253
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      1
_cell_measurement_theta_min      10
_cell_volume                     1681.91(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.063
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6896
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         29.8
_diffrn_reflns_theta_min         2.8
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    8.428
_exptl_absorpt_correction_T_max  0.2835
_exptl_absorpt_correction_T_min  0.2835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2008
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.83
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.401
_refine_diff_density_min         -2.34
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         4063
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0422P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                3196
_reflns_number_total             4063
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c4dt01143k1.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7031508--7031511.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7031510
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
C1 C 0.0534(4) 0.8830(6) 0.3678(4) 0.0225(12) Uani 1 1 d .
H1A H 0.0121 0.9093 0.4184 0.027 Uiso 1 1 calc R
H1B H 0.0741 0.7755 0.3767 0.027 Uiso 1 1 calc R
H1C H 0.0198 0.8955 0.3017 0.027 Uiso 1 1 calc R
C2 C 0.1064(4) 1.1597(5) 0.3654(4) 0.0209(12) Uani 1 1 d .
H2A H 0.0735 1.1902 0.4222 0.025 Uiso 1 1 calc R
H2B H 0.0644 1.1697 0.3042 0.025 Uiso 1 1 calc R
H2C H 0.1606 1.2269 0.3617 0.025 Uiso 1 1 calc R
C3 C 0.1876(4) 0.9726(6) 0.4821(4) 0.0197(11) Uani 1 1 d .
H3A H 0.1427 0.9876 0.5308 0.024 Uiso 1 1 calc R
H3B H 0.2374 1.0496 0.493 0.024 Uiso 1 1 calc R
H3C H 0.2144 0.8685 0.4895 0.024 Uiso 1 1 calc R
C4 C 0.1387(3) 0.9910(5) 0.3781(4) 0.0129(10) Uani 1 1 d .
C5 C 0.1031(4) 0.9050(7) 0.1178(4) 0.0271(13) Uani 1 1 d .
H5A H 0.0918 0.9289 0.0469 0.033 Uiso 1 1 calc R
H5B H 0.0509 0.9429 0.152 0.033 Uiso 1 1 calc R
H5C H 0.109 0.7928 0.1267 0.033 Uiso 1 1 calc R
C6 C 0.1848(4) 1.1577(6) 0.1439(4) 0.0235(12) Uani 1 1 d .
H6A H 0.1884 1.1802 0.0735 0.028 Uiso 1 1 calc R
H6B H 0.2358 1.2104 0.1838 0.028 Uiso 1 1 calc R
H6C H 0.1251 1.1943 0.1634 0.028 Uiso 1 1 calc R
C7 C 0.2755(4) 0.9226(6) 0.1073(4) 0.0227(12) Uani 1 1 d .
H7A H 0.2605 0.9325 0.0354 0.027 Uiso 1 1 calc R
H7B H 0.2869 0.8136 0.1244 0.027 Uiso 1 1 calc R
H7C H 0.3315 0.9833 0.1282 0.027 Uiso 1 1 calc R
C8 C 0.1929(3) 0.9834(6) 0.1610(4) 0.0147(11) Uani 1 1 d .
C9 C 0.4055(4) 0.9754(6) 0.3502(4) 0.0159(11) Uani 1 1 d .
C10 C 0.4849(3) 1.0697(6) 0.3652(4) 0.0191(11) Uani 1 1 d .
H10 H 0.4797 1.1787 0.3579 0.023 Uiso 1 1 calc R
C11 C 0.5692(4) 1.0028(6) 0.3903(4) 0.0217(12) Uani 1 1 d .
H11 H 0.6236 1.0648 0.4008 0.026 Uiso 1 1 calc R
C12 C 0.5752(4) 0.8432(7) 0.4005(4) 0.0261(13) Uani 1 1 d .
H12 H 0.6334 0.7948 0.4193 0.031 Uiso 1 1 calc R
C13 C 0.4957(4) 0.7570(7) 0.3829(4) 0.0219(12) Uani 1 1 d .
H13 H 0.5007 0.6476 0.3881 0.026 Uiso 1 1 calc R
C14 C 0.1680(4) 0.5632(6) 0.2856(4) 0.0252(13) Uani 1 1 d .
H14A H 0.1817 0.4791 0.2407 0.03 Uiso 1 1 calc R
H14B H 0.1199 0.6305 0.2524 0.03 Uiso 1 1 calc R
H14C H 0.1458 0.5196 0.3456 0.03 Uiso 1 1 calc R
C15 C 0.3497(4) 0.4735(6) 0.3598(4) 0.0203(12) Uani 1 1 d .
H15A H 0.3823 0.437 0.3042 0.024 Uiso 1 1 calc R
H15B H 0.3019 0.3981 0.3734 0.024 Uiso 1 1 calc R
H15C H 0.3944 0.4854 0.4188 0.024 Uiso 1 1 calc R
N1 N 0.3184(3) 1.0394(4) 0.3258(3) 0.0130(8) Uani 1 1 d U
H1 H 0.3113 1.1404 0.3275 0.016 Uiso 1 1 calc R
N2 N 0.4102(3) 0.8196(5) 0.3585(3) 0.0163(9) Uani 1 1 d .
P1 P 0.22452(9) 0.92405(15) 0.29260(9) 0.0120(3) Uani 1 1 d .
Pt1 Pt 0.286134(13) 0.68878(2) 0.323066(14) 0.01369(8) Uani 1 1 d .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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
C4 C1 H1A 109.5
C4 C1 H1B 109.5
H1A C1 H1B 109.5
C4 C1 H1C 109.5
H1A C1 H1C 109.5
H1B C1 H1C 109.5
C4 C2 H2A 109.5
C4 C2 H2B 109.5
H2A C2 H2B 109.5
C4 C2 H2C 109.5
H2A C2 H2C 109.5
H2B C2 H2C 109.5
C4 C3 H3A 109.5
C4 C3 H3B 109.5
H3A C3 H3B 109.5
C4 C3 H3C 109.5
H3A C3 H3C 109.5
H3B C3 H3C 109.5
C3 C4 C2 108.1(4)
C3 C4 C1 108.2(4)
C2 C4 C1 109.6(4)
C3 C4 P1 105.5(3)
C2 C4 P1 115.9(3)
C1 C4 P1 109.2(3)
C8 C5 H5A 109.5
C8 C5 H5B 109.5
H5A C5 H5B 109.5
C8 C5 H5C 109.5
H5A C5 H5C 109.5
H5B C5 H5C 109.5
C8 C6 H6A 109.5
C8 C6 H6B 109.5
H6A C6 H6B 109.5
C8 C6 H6C 109.5
H6A C6 H6C 109.5
H6B C6 H6C 109.5
C8 C7 H7A 109.5
C8 C7 H7B 109.5
H7A C7 H7B 109.5
C8 C7 H7C 109.5
H7A C7 H7C 109.5
H7B C7 H7C 109.5
C5 C8 C6 109.3(5)
C5 C8 C7 109.4(4)
C6 C8 C7 108.3(4)
C5 C8 P1 111.1(4)
C6 C8 P1 115.1(4)
C7 C8 P1 103.3(4)
N2 C9 N1 117.1(5)
N2 C9 C10 122.2(5)
N1 C9 C10 120.8(5)
C11 C10 C9 119.1(5)
C11 C10 H10 120.5
C9 C10 H10 120.5
C10 C11 C12 119.6(5)
C10 C11 H11 120.2
C12 C11 H11 120.2
C13 C12 C11 118.8(6)
C13 C12 H12 120.6
C11 C12 H12 120.6
N2 C13 C12 123.4(5)
N2 C13 H13 118.3
C12 C13 H13 118.3
Pt1 C14 H14A 109.5
Pt1 C14 H14B 109.5
H14A C14 H14B 109.5
Pt1 C14 H14C 109.5
H14A C14 H14C 109.5
H14B C14 H14C 109.5
Pt1 C15 H15A 109.5
Pt1 C15 H15B 109.5
H15A C15 H15B 109.5
Pt1 C15 H15C 109.5
H15A C15 H15C 109.5
H15B C15 H15C 109.5
C9 N1 P1 120.5(3)
C9 N1 H1 119.7
P1 N1 H1 119.7
C9 N2 C13 117.0(5)
C9 N2 Pt1 118.4(4)
C13 N2 Pt1 124.4(3)
N1 P1 C8 101.7(2)
N1 P1 C4 102.3(2)
C8 P1 C4 113.2(2)
N1 P1 Pt1 101.08(14)
C8 P1 Pt1 118.64(16)
C4 P1 Pt1 116.20(15)
C14 Pt1 C15 85.5(2)
C14 Pt1 N2 178.58(19)
C15 Pt1 N2 94.56(18)
C14 Pt1 P1 97.54(15)
C15 Pt1 P1 176.21(16)
N2 Pt1 P1 82.44(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C4 1.539(7)
C1 H1A 0.98
C1 H1B 0.98
C1 H1C 0.98
C2 C4 1.535(6)
C2 H2A 0.98
C2 H2B 0.98
C2 H2C 0.98
C3 C4 1.519(7)
C3 H3A 0.98
C3 H3B 0.98
C3 H3C 0.98
C4 P1 1.872(5)
C5 C8 1.526(7)
C5 H5A 0.98
C5 H5B 0.98
C5 H5C 0.98
C6 C8 1.526(7)
C6 H6A 0.98
C6 H6B 0.98
C6 H6C 0.98
C7 C8 1.551(7)
C7 H7A 0.98
C7 H7B 0.98
C7 H7C 0.98
C8 P1 1.867(5)
C9 N2 1.353(6)
C9 N1 1.382(6)
C9 C10 1.404(7)
C10 C11 1.358(7)
C10 H10 0.95
C11 C12 1.388(7)
C11 H11 0.95
C12 C13 1.368(8)
C12 H12 0.95
C13 N2 1.358(7)
C13 H13 0.95
C14 Pt1 2.041(5)
C14 H14A 0.98
C14 H14B 0.98
C14 H14C 0.98
C15 Pt1 2.112(5)
C15 H15A 0.98
C15 H15B 0.98
C15 H15C 0.98
N1 P1 1.705(4)
N1 H1 0.88
N2 Pt1 2.131(4)
P1 Pt1 2.2411(13)
