#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:53:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179352 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/49/4324999.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_4324999
loop_
_publ_author_name
'Joanna R. Webb'
'Colleen Munro-Leighton'
'Aaron W. Pierpont'
'Joshua T. Gurkin'
'T. Brent Gunnoe'
'Thomas R. Cundari'
'Michal Sabat'
'Jeffrey L. Petersen'
'Paul D. Boyle'
_publ_contact_author_address
;University of Virginia
Charlottesville VA 22904
;
_publ_contact_author_email       tbg7h@virginia.edu
_publ_contact_author_name        'T. Brent Gunnoe'
_publ_contact_author_phone       434-982-2692
_publ_section_title
;
 Pt(II) and Pt(IV) Amido, Aryloxide, and Hydrocarbyl Complexes: Synthesis,
 Characterization, and Reaction with Dihydrogen and Substrates that
 Possess C-H Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4195
_journal_page_last               4211
_journal_paper_doi               10.1021/ic200153n
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C30 H36 N4 Pt'
_chemical_formula_weight         647.72
_chemical_name_systematic
; 
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.474(3)
_cell_angle_beta                 72.801(3)
_cell_angle_gamma                87.372(3)
_cell_formula_units_Z            2
_cell_length_a                   8.6069(14)
_cell_length_b                   12.698(2)
_cell_length_c                   13.618(2)
_cell_measurement_reflns_used    7539
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      29.871
_cell_measurement_theta_min      2.480
_cell_volume                     1354.2(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker SMART APEX 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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0871
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18198
_diffrn_reflns_theta_full        32.58
_diffrn_reflns_theta_max         32.58
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    5.205
_exptl_absorpt_correction_T_max  0.801936
_exptl_absorpt_correction_T_min  0.587551
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_meas      0
_exptl_crystal_description       plate
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.809
_refine_diff_density_min         -1.450
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         9512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0245P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                7104
_reflns_number_total             9512
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200153n_si_002_3.cif
_cod_data_source_block           C30H36N4Pt
_cod_database_code               4324999
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
Pt Pt 0.73676(2) 0.415450(17) 1.057869(15) 0.03530(6) Uani 1 1 d .
N1 N 0.6430(5) 0.3366(3) 0.9777(3) 0.0342(9) Uani 1 1 d .
N2 N 0.7256(5) 0.5427(3) 0.9296(3) 0.0326(8) Uani 1 1 d .
N3 N 0.8362(6) 0.5099(4) 1.1189(4) 0.0446(11) Uani 1 1 d .
N4 N 0.7494(7) 0.2791(5) 1.1736(4) 0.0515(14) Uani 1 1 d .
C1 C 0.5938(7) 0.2299(5) 1.0119(4) 0.0427(12) Uani 1 1 d .
C2 C 0.5475(7) 0.1804(5) 0.9471(5) 0.0441(13) Uani 1 1 d .
C3 C 0.5475(6) 0.2394(4) 0.8437(4) 0.0360(11) Uani 1 1 d .
C4 C 0.5898(6) 0.3518(4) 0.8122(4) 0.0377(11) Uani 1 1 d .
C5 C 0.6372(6) 0.3985(4) 0.8787(4) 0.0345(10) Uani 1 1 d .
C6 C 0.6878(6) 0.5160(4) 0.8502(4) 0.0317(10) Uani 1 1 d .
C7 C 0.7007(6) 0.5930(4) 0.7517(4) 0.0340(10) Uani 1 1 d .
C8 C 0.7494(6) 0.7023(4) 0.7297(4) 0.0375(11) Uani 1 1 d .
C9 C 0.7814(7) 0.7278(5) 0.8146(5) 0.0440(13) Uani 1 1 d .
C10 C 0.7692(7) 0.6492(5) 0.9107(4) 0.0422(12) Uani 1 1 d .
C11 C 0.5063(7) 0.1872(4) 0.7675(4) 0.0431(12) Uani 1 1 d .
C12 C 0.4633(8) 0.0627(4) 0.8185(5) 0.0557(16) Uani 1 1 d .
H12A H 0.5530 0.0263 0.8407 0.084 Uiso 1 1 calc R
H12B H 0.4416 0.0330 0.7666 0.084 Uiso 1 1 calc R
H12C H 0.3686 0.0509 0.8800 0.084 Uiso 1 1 calc R
C13 C 0.6551(9) 0.2036(5) 0.6679(5) 0.0688(19) Uani 1 1 d .
H13A H 0.6825 0.2811 0.6342 0.103 Uiso 1 1 calc R
H13B H 0.6304 0.1724 0.6179 0.103 Uiso 1 1 calc R
H13C H 0.7455 0.1674 0.6893 0.103 Uiso 1 1 calc R
C14 C 0.3595(9) 0.2424(5) 0.7349(6) 0.071(2) Uani 1 1 d .
H14A H 0.2682 0.2337 0.7982 0.107 Uiso 1 1 calc R
H14B H 0.3323 0.2085 0.6876 0.107 Uiso 1 1 calc R
H14C H 0.3860 0.3197 0.6985 0.107 Uiso 1 1 calc R
C15 C 0.7799(7) 0.7872(4) 0.6180(4) 0.0440(13) Uani 1 1 d .
C16 C 0.7318(13) 0.9009(6) 0.6292(7) 0.115(4) Uani 1 1 d .
H16A H 0.7492 0.9532 0.5589 0.172 Uiso 1 1 calc R
H16B H 0.7971 0.9235 0.6662 0.172 Uiso 1 1 calc R
H16C H 0.6189 0.8976 0.6695 0.172 Uiso 1 1 calc R
C17 C 0.9601(9) 0.7928(9) 0.5614(7) 0.122(4) Uani 1 1 d .
H17A H 0.9936 0.7208 0.5569 0.184 Uiso 1 1 calc R
H17B H 1.0187 0.8172 0.6012 0.184 Uiso 1 1 calc R
H17C H 0.9829 0.8438 0.4901 0.184 Uiso 1 1 calc R
C18 C 0.6845(11) 0.7591(6) 0.5539(6) 0.100(3) Uani 1 1 d .
H18A H 0.7164 0.6893 0.5423 0.150 Uiso 1 1 calc R
H18B H 0.7047 0.8155 0.4856 0.150 Uiso 1 1 calc R
H18C H 0.5705 0.7542 0.5923 0.150 Uiso 1 1 calc R
C19 C 0.8215(6) 0.5029(4) 1.2231(4) 0.0377(11) Uani 1 1 d .
C20 C 0.9355(7) 0.5569(5) 1.2494(5) 0.0451(13) Uani 1 1 d .
C21 C 0.9178(9) 0.5518(6) 1.3546(6) 0.0590(18) Uani 1 1 d .
C22 C 0.7871(10) 0.4946(6) 1.4374(5) 0.0616(18) Uani 1 1 d .
C23 C 0.6710(9) 0.4443(5) 1.4132(5) 0.0561(17) Uani 1 1 d .
C24 C 0.6870(7) 0.4499(5) 1.3091(4) 0.0431(13) Uani 1 1 d .
C25 C 0.8427(7) 0.1897(5) 1.1668(4) 0.0426(12) Uani 1 1 d .
C26 C 0.8411(9) 0.1006(5) 1.2583(5) 0.0554(16) Uani 1 1 d .
C27 C 0.9332(10) 0.0110(6) 1.2513(7) 0.069(2) Uani 1 1 d .
C28 C 1.0327(11) 0.0050(6) 1.1542(8) 0.077(2) Uani 1 1 d .
C29 C 1.0356(9) 0.0913(6) 1.0621(7) 0.0639(18) Uani 1 1 d .
C30 C 0.9416(8) 0.1814(5) 1.0688(5) 0.0487(14) Uani 1 1 d .
H1 H 0.600(6) 0.189(4) 1.081(4) 0.041(15) Uiso 1 1 d .
H1N3 H 0.933(7) 0.537(5) 1.076(5) 0.07(2) Uiso 1 1 d .
H1N4 H 0.724(7) 0.274(5) 1.225(4) 0.043(19) Uiso 1 1 d .
H2 H 0.522(6) 0.110(4) 0.969(4) 0.043(15) Uiso 1 1 d .
H4 H 0.595(5) 0.404(4) 0.744(4) 0.031(13) Uiso 1 1 d .
H7 H 0.682(5) 0.573(4) 0.702(4) 0.028(13) Uiso 1 1 d .
H9 H 0.817(6) 0.791(4) 0.802(4) 0.031(13) Uiso 1 1 d .
H10 H 0.789(5) 0.666(4) 0.967(4) 0.028(12) Uiso 1 1 d .
H20 H 1.027(6) 0.600(4) 1.199(4) 0.043(15) Uiso 1 1 d .
H21 H 0.988(6) 0.590(4) 1.360(4) 0.039(16) Uiso 1 1 d .
H22 H 0.786(8) 0.490(5) 1.504(5) 0.07(2) Uiso 1 1 d .
H23 H 0.586(9) 0.408(6) 1.470(6) 0.10(3) Uiso 1 1 d .
H24 H 0.612(6) 0.419(5) 1.294(4) 0.050(17) Uiso 1 1 d .
H26 H 0.770(6) 0.092(4) 1.321(4) 0.041(16) Uiso 1 1 d .
H27 H 0.926(7) -0.041(5) 1.312(5) 0.07(2) Uiso 1 1 d .
H28 H 1.099(9) -0.053(6) 1.149(6) 0.09(3) Uiso 1 1 d .
H29 H 1.109(7) 0.091(5) 0.990(5) 0.07(2) Uiso 1 1 d .
H30 H 0.943(6) 0.234(4) 1.011(4) 0.033(14) Uiso 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'
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'
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
N4 Pt N3 92.5(2)
N4 Pt N2 173.48(19)
N3 Pt N2 93.28(18)
N4 Pt N1 94.8(2)
N3 Pt N1 172.42(17)
N2 Pt N1 79.35(16)
C1 N1 C5 118.4(4)
C1 N1 Pt 126.0(4)
C5 N1 Pt 115.6(3)
C10 N2 C6 117.4(4)
C10 N2 Pt 126.1(4)
C6 N2 Pt 116.1(3)
C19 N3 Pt 130.7(4)
C25 N4 Pt 129.2(4)
N1 C1 C2 122.0(5)
C1 C2 C3 121.4(5)
C2 C3 C4 115.7(5)
C2 C3 C11 123.2(4)
C4 C3 C11 121.1(4)
C5 C4 C3 121.4(5)
N1 C5 C4 121.1(4)
N1 C5 C6 114.3(4)
C4 C5 C6 124.6(4)
N2 C6 C7 121.7(4)
N2 C6 C5 113.8(4)
C7 C6 C5 124.6(4)
C6 C7 C8 121.8(5)
C7 C8 C9 115.0(5)
C7 C8 C15 122.9(5)
C9 C8 C15 121.9(5)
C10 C9 C8 121.7(5)
N2 C10 C9 122.4(5)
C3 C11 C14 109.5(5)
C3 C11 C13 108.2(5)
C14 C11 C13 110.3(5)
C3 C11 C12 112.6(4)
C14 C11 C12 107.9(5)
C13 C11 C12 108.3(5)
C18 C15 C17 111.0(7)
C18 C15 C16 107.6(6)
C17 C15 C16 108.4(7)
C18 C15 C8 112.3(5)
C17 C15 C8 107.4(5)
C16 C15 C8 110.0(5)
N3 C19 C24 122.6(5)
N3 C19 C20 121.3(5)
C24 C19 C20 115.8(5)
C21 C20 C19 121.1(6)
C20 C21 C22 121.1(6)
C21 C22 C23 118.8(6)
C24 C23 C22 120.3(7)
C23 C24 C19 122.7(6)
N4 C25 C30 121.7(5)
N4 C25 C26 121.9(6)
C30 C25 C26 116.3(6)
C27 C26 C25 121.9(7)
C26 C27 C28 121.1(7)
C27 C28 C29 118.4(7)
C30 C29 C28 120.6(8)
C29 C30 C25 121.7(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pt N4 1.984(5)
Pt N3 1.995(4)
Pt N2 2.014(4)
Pt N1 2.024(4)
N1 C1 1.337(6)
N1 C5 1.355(6)
N2 C10 1.348(7)
N2 C6 1.352(6)
N3 C19 1.362(6)
N4 C25 1.371(7)
C1 C2 1.377(7)
C2 C3 1.382(7)
C3 C4 1.392(7)
C3 C11 1.515(7)
C4 C5 1.380(7)
C5 C6 1.476(6)
C6 C7 1.378(6)
C7 C8 1.386(7)
C8 C9 1.393(7)
C8 C15 1.532(7)
C9 C10 1.364(7)
C11 C14 1.533(8)
C11 C13 1.534(8)
C11 C12 1.535(7)
C15 C18 1.484(8)
C15 C17 1.509(9)
C15 C16 1.522(9)
C19 C24 1.400(7)
C19 C20 1.406(7)
C20 C21 1.376(8)
C21 C22 1.377(10)
C22 C23 1.377(9)
C23 C24 1.363(8)
C25 C30 1.386(8)
C25 C26 1.405(8)
C26 C27 1.367(10)
C27 C28 1.369(11)
C28 C29 1.390(10)
C29 C30 1.380(9)
