# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material 
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#  disseminated in any form, whether machine-readable or not,  
#  except for the purpose of generating routine backup copies 
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#  data retrieval see:
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#  Bona fide researchers may freely download Mercury and enCIFer
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data_E2a
_database_code_depnum_ccdc_archive 'CCDC 904374'
#TrackingRef 'web_deposit_cif_file_0_ConcettaPacifico_1349943769.all.cif'
_audit_creation_method           SHELXL-97
_audit_creation_date             05-08-16
_exptl_crystal_recrystallization_method 
;
>From CH2Cl2/hexane
;
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Pt(Me2NCH2CH2NMe2)(C8H7)Cl]'
_chemical_formula_sum            'C14 H23 Cl N2 Pt'
_chemical_formula_weight         449.88
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'
Cl Cl 0.1484 0.1585 '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'
_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, -z'
'-x, y-1/2, -z-1/2'
'x-1/2, y, -z-1/2'
_cell_length_a                   21.7511(17)
_cell_length_b                   11.4643(9)
_cell_length_c                   37.772(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     9418.8(13)
_cell_formula_units_Z            24
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6709
_cell_measurement_theta_min      2
_cell_measurement_theta_max      27.5
_exptl_crystal_description       lath
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5184
_exptl_absorpt_coefficient_mu    9.095
_exptl_absorpt_correction_type   'Integration + multiscan'
_exptl_absorpt_correction_T_min  0.01975
_exptl_absorpt_correction_T_max  0.29063
_exptl_absorpt_process_details   'XPREP + SADABS'
_exptl_special_details           
;
Oxford crysosystems lt device
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       Omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            135583
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_theta_min         1.08
_diffrn_reflns_theta_max         28.97
_reflns_number_total             11993
_reflns_number_gt                10157
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       Smart
_computing_cell_refinement       Saint
_computing_data_reduction        Saint
_computing_structure_solution    Dirdif
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    XP
_computing_publication_material  'PLATON, XCIF'
_refine_special_details          
;
The crystals tended to separate out into shards when cut.
There are three molecules in the asymmetric unit. Symmetry checking does
not suggest a simpler description of the structure.
Checkcif output:
761_ALERT_1_A CIF Contains no X-H Bonds ...................... ?
762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ?
All idealised; no action.
063_ALERT_3_B Crystal Probably too Large for Beam Size ....... 0.90 mm
See above.
241_ALERT_2_B Check High Ueq as Compared to Neighbors for C11b
High thermal motion is not unusual in en-ligands. Here the max adp eigenvalue
is 0.1248, so no disorder modelling was deemed to be necessary.
242_ALERT_2_B Check Low Ueq as Compared to Neighbors for N1b
242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N2b
The terminal Me groups are librating (not unreasonable for this ligand) and
the N-atoms are 'pivots'.
912_ALERT_3_B # Missing FCF Reflections Above STH/L=0.6 ...... 501
The data collection strategy used aimed to achieve a complete data set to
2\q = 54 deg. Some higher angle data were collected in the process and these
have been included in the refinement.
#===============================================================================
Resolution & Completeness Statistics (Cumulative)
#===============================================================================
Theta sin(th)/Lambda Complete Expected Measured Missing
#-------------------------------------------------------------------------------
20.82 0.500 1.000 4936 4936 0
23.01 0.550 1.000 6563 6563 0
25.24 0.600 1.000 8519 8519 0
#----------------------------------------------------------- ACTA Min. Res. ----
27.51 0.650 1.000 10832 10832 0
28.97 0.682 0.960 12494 11993 501
094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.80
The difference map is noisey around the Pt-atoms.
220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.55 Ratio
222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.14 Ratio
042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
230_ALERT_2_C Hirshfeld Test Diff for C12b - C11b .. 5.23 su
795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C12a
797_ALERT_4_C N-Atom in CIF Coordinate List out of Sequence .. N2b
No action taken.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0154P)^2^+41.4919P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geometric
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11993
_refine_ls_number_parameters     487
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0687
_refine_ls_wR_factor_gt          0.0659
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
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
Pt1a Pt 0.203413(7) 0.106864(14) 0.498509(4) 0.01741(4) Uani 1 1 d . . .
Cl1a Cl 0.26812(5) 0.21600(10) 0.46364(3) 0.0255(2) Uani 1 1 d . . .
C8a C 0.1309(2) 0.1759(4) 0.47447(12) 0.0243(9) Uani 1 1 d . . .
H8a H 0.1173 0.2492 0.4832 0.029 Uiso 1 1 calc R . .
C7a C 0.0997(2) 0.1319(4) 0.44783(13) 0.0283(10) Uani 1 1 d . . .
H7a H 0.1150 0.0612 0.4381 0.034 Uiso 1 1 calc R . .
C1a C 0.0435(2) 0.1799(4) 0.43125(12) 0.0274(10) Uani 1 1 d . . .
C2a C 0.0136(2) 0.1137(5) 0.40570(13) 0.0317(11) Uani 1 1 d . . .
H2a H 0.0299 0.0398 0.3992 0.038 Uiso 1 1 calc R . .
C3a C -0.0398(2) 0.1537(5) 0.38937(14) 0.0380(13) Uani 1 1 d . . .
H3a H -0.0596 0.1069 0.3720 0.046 Uiso 1 1 calc R . .
C4a C -0.0640(2) 0.2604(5) 0.39819(15) 0.0403(14) Uani 1 1 d . . .
H4a H -0.1009 0.2875 0.3875 0.048 Uiso 1 1 calc R . .
C5a C -0.0337(2) 0.3270(5) 0.42292(16) 0.0405(13) Uani 1 1 d . . .
H5a H -0.0495 0.4018 0.4288 0.049 Uiso 1 1 calc R . .
C6a C 0.0189(2) 0.2881(5) 0.43935(14) 0.0324(11) Uani 1 1 d . . .
H6a H 0.0386 0.3361 0.4564 0.039 Uiso 1 1 calc R . .
N2a N 0.27935(17) 0.0227(3) 0.52531(10) 0.0216(8) Uani 1 1 d . . .
C12a C 0.2501(2) -0.0744(4) 0.54545(13) 0.0318(11) Uani 1 1 d . . .
H121a H 0.2781 -0.1012 0.5644 0.038 Uiso 1 1 calc R . .
H122a H 0.2420 -0.1409 0.5294 0.038 Uiso 1 1 calc R . .
C11a C 0.1909(2) -0.0326(5) 0.56130(12) 0.0321(11) Uani 1 1 d . . .
H111a H 0.1706 -0.0978 0.5739 0.039 Uiso 1 1 calc R . .
H112a H 0.1996 0.0297 0.5788 0.039 Uiso 1 1 calc R . .
N1a N 0.14895(17) 0.0134(3) 0.53328(10) 0.0239(8) Uani 1 1 d . . .
C14a C 0.3252(2) -0.0301(4) 0.50072(14) 0.0330(11) Uani 1 1 d . . .
H141a H 0.3043 -0.0848 0.4848 0.050 Uiso 1 1 calc R . .
H142a H 0.3565 -0.0717 0.5144 0.050 Uiso 1 1 calc R . .
H143a H 0.3448 0.0316 0.4868 0.050 Uiso 1 1 calc R . .
C13a C 0.3111(2) 0.1043(4) 0.54898(14) 0.0329(11) Uani 1 1 d . . .
H131a H 0.2813 0.1401 0.5651 0.049 Uiso 1 1 calc R . .
H132a H 0.3311 0.1653 0.5349 0.049 Uiso 1 1 calc R . .
H133a H 0.3422 0.0622 0.5627 0.049 Uiso 1 1 calc R . .
C9a C 0.1166(2) -0.0846(4) 0.51525(14) 0.0336(11) Uani 1 1 d . . .
H91a H 0.1469 -0.1353 0.5037 0.050 Uiso 1 1 calc R . .
H92a H 0.0884 -0.0533 0.4974 0.050 Uiso 1 1 calc R . .
H93a H 0.0933 -0.1297 0.5327 0.050 Uiso 1 1 calc R . .
C10a C 0.1023(2) 0.0876(5) 0.55059(14) 0.0360(12) Uani 1 1 d . . .
H101a H 0.1227 0.1529 0.5625 0.054 Uiso 1 1 calc R . .
H102a H 0.0795 0.0413 0.5680 0.054 Uiso 1 1 calc R . .
H103a H 0.0738 0.1178 0.5327 0.054 Uiso 1 1 calc R . .
Pt1b Pt 0.712148(8) 0.084196(16) 0.671383(4) 0.02117(5) Uani 1 1 d . . .
Cl1b Cl 0.68667(6) 0.20217(12) 0.71857(3) 0.0348(3) Uani 1 1 d . . .
C8b C 0.7995(2) 0.0764(5) 0.68627(13) 0.0315(11) Uani 1 1 d . . .
H8b H 0.8159 -0.0003 0.6869 0.038 Uiso 1 1 calc R . .
C7b C 0.8390(2) 0.1585(5) 0.69553(12) 0.0295(11) Uani 1 1 d . . .
H7b H 0.8248 0.2369 0.6959 0.035 Uiso 1 1 calc R . .
C1b C 0.9039(2) 0.1367(5) 0.70542(12) 0.0292(11) Uani 1 1 d . . .
C2b C 0.9337(2) 0.2156(5) 0.72773(13) 0.0343(12) Uani 1 1 d . . .
H2b H 0.9127 0.2837 0.7355 0.041 Uiso 1 1 calc R . .
C3b C 0.9938(2) 0.1959(6) 0.73875(14) 0.0405(13) Uani 1 1 d . . .
H3b H 1.0128 0.2493 0.7546 0.049 Uiso 1 1 calc R . .
C4b C 1.0260(3) 0.1002(6) 0.72707(14) 0.0426(14) Uani 1 1 d . . .
H4b H 1.0674 0.0885 0.7342 0.051 Uiso 1 1 calc R . .
C5b C 0.9975(2) 0.0213(5) 0.70499(14) 0.0403(13) Uani 1 1 d . . .
H73 H 1.0191 -0.0457 0.6971 0.048 Uiso 1 1 calc R . .
C6b C 0.9368(2) 0.0399(5) 0.69423(13) 0.0369(12) Uani 1 1 d . . .
H6b H 0.9177 -0.0150 0.6789 0.044 Uiso 1 1 calc R . .
N2b N 0.61658(19) 0.0768(4) 0.65368(11) 0.0310(9) Uani 1 1 d . . .
C12b C 0.6189(3) 0.0210(6) 0.61852(15) 0.0429(14) Uani 1 1 d . . .
H121b H 0.5799 -0.0214 0.6145 0.051 Uiso 1 1 calc R . .
H122b H 0.6221 0.0826 0.6002 0.051 Uiso 1 1 calc R . .
C11b C 0.6697(3) -0.0596(7) 0.61411(19) 0.066(2) Uani 1 1 d . . .
H111b H 0.6730 -0.0804 0.5887 0.079 Uiso 1 1 calc R . .
H112b H 0.6604 -0.1319 0.6274 0.079 Uiso 1 1 calc R . .
N1b N 0.72961(17) -0.0135(3) 0.62627(9) 0.0234(8) Uani 1 1 d . . .
C13b C 0.5873(3) 0.1914(6) 0.65085(18) 0.0571(19) Uani 1 1 d . . .
H131b H 0.6113 0.2409 0.6349 0.086 Uiso 1 1 calc R . .
H132b H 0.5855 0.2277 0.6743 0.086 Uiso 1 1 calc R . .
H133b H 0.5456 0.1823 0.6415 0.086 Uiso 1 1 calc R . .
C14b C 0.5805(3) 0.0027(8) 0.67772(18) 0.068(2) Uani 1 1 d . . .
H141b H 0.6003 -0.0738 0.6798 0.102 Uiso 1 1 calc R . .
H142b H 0.5389 -0.0071 0.6682 0.102 Uiso 1 1 calc R . .
H143b H 0.5783 0.0395 0.7011 0.102 Uiso 1 1 calc R . .
C10b C 0.7689(4) -0.1179(6) 0.63167(17) 0.074(3) Uani 1 1 d . . .
H101b H 0.7504 -0.1679 0.6498 0.110 Uiso 1 1 calc R . .
H102b H 0.8099 -0.0933 0.6394 0.110 Uiso 1 1 calc R . .
H103b H 0.7721 -0.1613 0.6094 0.110 Uiso 1 1 calc R . .
C9b C 0.7604(4) 0.0556(6) 0.59947(14) 0.062(2) Uani 1 1 d . . .
H91b H 0.7991 0.0859 0.6090 0.093 Uiso 1 1 calc R . .
H92b H 0.7339 0.1209 0.5925 0.093 Uiso 1 1 calc R . .
H93b H 0.7689 0.0068 0.5787 0.093 Uiso 1 1 calc R . .
Pt1c Pt 0.197767(7) 0.138454(15) 0.162517(4) 0.01786(4) Uani 1 1 d . . .
Cl1c Cl 0.25860(5) 0.25246(10) 0.12663(3) 0.0257(2) Uani 1 1 d . . .
C8c C 0.1219(2) 0.2013(4) 0.14092(12) 0.0219(9) Uani 1 1 d . . .
H8c H 0.1057 0.2699 0.1515 0.026 Uiso 1 1 calc R . .
C7c C 0.0907(2) 0.1595(4) 0.11343(12) 0.0258(10) Uani 1 1 d . . .
H7c H 0.1091 0.0965 0.1010 0.031 Uiso 1 1 calc R . .
C1c C 0.0307(2) 0.2004(4) 0.10011(12) 0.0236(9) Uani 1 1 d . . .
C6c C -0.0100(2) 0.2644(4) 0.12128(13) 0.0279(10) Uani 1 1 d . . .
H6c H 0.0007 0.2819 0.1451 0.033 Uiso 1 1 calc R . .
C5c C -0.0655(2) 0.3023(5) 0.10791(14) 0.0311(11) Uani 1 1 d . . .
H5c H -0.0922 0.3466 0.1226 0.037 Uiso 1 1 calc R . .
C4c C -0.0831(2) 0.2770(5) 0.07365(14) 0.0352(12) Uani 1 1 d . . .
H4c H -0.1213 0.3041 0.0647 0.042 Uiso 1 1 calc R . .
C3c C -0.0445(2) 0.2121(5) 0.05261(14) 0.0350(12) Uani 1 1 d . . .
H3c H -0.0563 0.1936 0.0290 0.042 Uiso 1 1 calc R . .
C2c C 0.0121(2) 0.1731(4) 0.06581(13) 0.0298(11) Uani 1 1 d . . .
H2c H 0.0381 0.1274 0.0511 0.036 Uiso 1 1 calc R . .
N2c N 0.27669(17) 0.0586(3) 0.18858(10) 0.0230(8) Uani 1 1 d . . .
C12c C 0.2504(2) -0.0431(4) 0.20745(12) 0.0274(10) Uani 1 1 d . . .
H121c H 0.2791 -0.0690 0.2262 0.033 Uiso 1 1 calc R . .
H122c H 0.2445 -0.1085 0.1907 0.033 Uiso 1 1 calc R . .
C11c C 0.1894(2) -0.0103(4) 0.22374(12) 0.0275(10) Uani 1 1 d . . .
H111c H 0.1712 -0.0794 0.2355 0.033 Uiso 1 1 calc R . .
H112c H 0.1958 0.0507 0.2419 0.033 Uiso 1 1 calc R . .
N1c N 0.14644(17) 0.0339(3) 0.19611(10) 0.0227(8) Uani 1 1 d . . .
C14c C 0.3048(3) 0.1408(5) 0.21421(14) 0.0357(12) Uani 1 1 d . . .
H141c H 0.2734 0.1682 0.2308 0.053 Uiso 1 1 calc R . .
H142c H 0.3222 0.2075 0.2014 0.053 Uiso 1 1 calc R . .
H143c H 0.3376 0.1009 0.2273 0.053 Uiso 1 1 calc R . .
C13c C 0.3241(2) 0.0174(5) 0.16402(13) 0.0308(11) Uani 1 1 d . . .
H131c H 0.3418 0.0841 0.1514 0.046 Uiso 1 1 calc R . .
H132c H 0.3057 -0.0367 0.1470 0.046 Uiso 1 1 calc R . .
H133c H 0.3565 -0.0227 0.1773 0.046 Uiso 1 1 calc R . .
C10c C 0.0961(2) 0.0972(5) 0.21443(14) 0.0342(12) Uani 1 1 d . . .
H101c H 0.0669 0.1271 0.1969 0.051 Uiso 1 1 calc R . .
H102c H 0.1134 0.1625 0.2279 0.051 Uiso 1 1 calc R . .
H103c H 0.0749 0.0439 0.2306 0.051 Uiso 1 1 calc R . .
C9c C 0.1193(2) -0.0655(4) 0.17660(13) 0.0276(10) Uani 1 1 d . . .
H91c H 0.0912 -0.0361 0.1584 0.041 Uiso 1 1 calc R . .
H92c H 0.0966 -0.1154 0.1931 0.041 Uiso 1 1 calc R . .
H93c H 0.1522 -0.1108 0.1654 0.041 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1a 0.02003(8) 0.01598(8) 0.01622(8) 0.00005(6) -0.00055(6) -0.00005(6)
Cl1a 0.0298(6) 0.0249(6) 0.0218(5) 0.0013(4) 0.0046(4) -0.0035(4)
C8a 0.022(2) 0.020(2) 0.031(2) 0.0047(19) -0.0006(18) 0.0000(18)
C7a 0.028(2) 0.025(3) 0.032(2) -0.001(2) -0.0024(19) 0.007(2)
C1a 0.023(2) 0.032(3) 0.027(2) 0.007(2) -0.0015(18) 0.002(2)
C2a 0.032(3) 0.030(3) 0.033(3) 0.006(2) -0.003(2) -0.002(2)
C3a 0.028(3) 0.055(4) 0.031(3) 0.013(3) -0.006(2) -0.014(3)
C4a 0.020(2) 0.054(4) 0.047(3) 0.029(3) -0.004(2) -0.002(2)
C5a 0.030(3) 0.038(3) 0.054(3) 0.014(3) 0.004(2) 0.007(2)
C6a 0.027(3) 0.033(3) 0.037(3) 0.006(2) 0.001(2) 0.000(2)
N2a 0.0251(19) 0.0165(19) 0.0234(18) -0.0010(15) -0.0015(15) -0.0004(15)
C12a 0.036(3) 0.029(3) 0.031(2) 0.007(2) -0.003(2) 0.001(2)
C11a 0.042(3) 0.032(3) 0.022(2) 0.007(2) 0.002(2) -0.002(2)
N1a 0.0248(19) 0.024(2) 0.0232(18) 0.0006(16) 0.0061(15) -0.0011(16)
C14a 0.030(3) 0.028(3) 0.041(3) -0.007(2) -0.004(2) 0.008(2)
C13a 0.039(3) 0.025(3) 0.035(3) -0.005(2) -0.014(2) 0.002(2)
C9a 0.041(3) 0.027(3) 0.034(3) 0.002(2) -0.001(2) -0.009(2)
C10a 0.036(3) 0.036(3) 0.036(3) 0.000(2) 0.018(2) 0.005(2)
Pt1b 0.02586(9) 0.02192(9) 0.01574(8) 0.00150(6) -0.00255(6) 0.00197(7)
Cl1b 0.0465(7) 0.0369(7) 0.0210(5) -0.0055(5) -0.0043(5) 0.0119(6)
C8b 0.030(3) 0.034(3) 0.030(2) -0.002(2) -0.001(2) 0.004(2)
C7b 0.033(3) 0.031(3) 0.024(2) 0.001(2) 0.0031(19) 0.001(2)
C1b 0.028(2) 0.040(3) 0.019(2) 0.005(2) 0.0012(18) -0.007(2)
C2b 0.035(3) 0.039(3) 0.028(3) 0.003(2) 0.004(2) -0.005(2)
C3b 0.031(3) 0.055(4) 0.035(3) 0.005(3) 0.000(2) -0.015(3)
C4b 0.028(3) 0.066(4) 0.034(3) 0.014(3) 0.001(2) -0.004(3)
C5b 0.034(3) 0.053(4) 0.034(3) 0.008(3) 0.008(2) 0.003(3)
C6b 0.034(3) 0.049(3) 0.028(3) 0.000(2) 0.001(2) -0.001(2)
N2b 0.025(2) 0.038(3) 0.030(2) 0.0000(19) -0.0050(17) 0.0037(18)
C12b 0.034(3) 0.053(4) 0.042(3) -0.015(3) -0.012(2) 0.004(3)
C11b 0.042(4) 0.096(6) 0.059(4) -0.043(4) -0.006(3) -0.009(4)
N1b 0.0244(19) 0.025(2) 0.0204(18) 0.0002(15) 0.0008(15) -0.0019(16)
C13b 0.055(4) 0.056(4) 0.060(4) -0.027(3) -0.028(3) 0.032(3)
C14b 0.036(3) 0.116(7) 0.052(4) 0.025(4) 0.002(3) -0.025(4)
C10b 0.146(8) 0.036(4) 0.039(3) -0.009(3) -0.015(4) 0.032(4)
C9b 0.102(6) 0.059(4) 0.026(3) -0.016(3) 0.029(3) -0.040(4)
Pt1c 0.02029(8) 0.01747(9) 0.01582(8) 0.00060(6) -0.00034(6) 0.00003(6)
Cl1c 0.0318(6) 0.0236(6) 0.0219(5) 0.0020(4) 0.0042(4) -0.0041(5)
C8c 0.022(2) 0.018(2) 0.025(2) 0.0033(17) -0.0012(17) 0.0004(17)
C7c 0.027(2) 0.026(3) 0.025(2) -0.0020(19) 0.0010(18) 0.0029(19)
C1c 0.025(2) 0.020(2) 0.026(2) 0.0038(18) -0.0010(18) -0.0041(18)
C6c 0.026(2) 0.029(3) 0.029(2) 0.004(2) -0.0027(19) -0.001(2)
C5c 0.024(2) 0.030(3) 0.039(3) 0.004(2) -0.002(2) -0.002(2)
C4c 0.026(3) 0.037(3) 0.043(3) 0.008(2) -0.010(2) -0.002(2)
C3c 0.035(3) 0.040(3) 0.031(3) 0.004(2) -0.012(2) -0.007(2)
C2c 0.034(3) 0.028(3) 0.028(2) 0.000(2) -0.003(2) -0.004(2)
N2c 0.0235(19) 0.021(2) 0.0247(19) -0.0004(15) -0.0060(15) 0.0004(15)
C12c 0.032(2) 0.024(2) 0.027(2) 0.0067(19) -0.004(2) -0.001(2)
C11c 0.033(3) 0.030(3) 0.020(2) 0.0042(19) 0.0014(19) 0.000(2)
N1c 0.0241(19) 0.020(2) 0.0237(18) 0.0028(15) 0.0066(15) 0.0012(15)
C14c 0.041(3) 0.032(3) 0.034(3) -0.004(2) -0.014(2) -0.004(2)
C13c 0.025(2) 0.033(3) 0.034(3) 0.004(2) 0.002(2) 0.006(2)
C10c 0.034(3) 0.031(3) 0.038(3) -0.002(2) 0.011(2) 0.003(2)
C9c 0.028(2) 0.024(2) 0.031(2) 0.001(2) 0.0001(19) -0.0029(19)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Pt1a C8a 1.984(4) . ?
Pt1a N1a 2.068(4) . ?
Pt1a N2a 2.164(4) . ?
Pt1a Cl1a 2.2979(11) . ?
C8a C7a 1.315(7) . ?
C7a C1a 1.479(6) . ?
C1a C6a 1.386(7) . ?
C1a C2a 1.390(7) . ?
C2a C3a 1.393(7) . ?
C3a C4a 1.373(8) . ?
C4a C5a 1.375(8) . ?
C5a C6a 1.377(7) . ?
N2a C13a 1.467(6) . ?
N2a C14a 1.490(6) . ?
N2a C12a 1.491(6) . ?
C12a C11a 1.498(7) . ?
C11a N1a 1.494(6) . ?
N1a C10a 1.476(6) . ?
N1a C9a 1.491(6) . ?
Pt1b C8b 1.983(5) . ?
Pt1b N1b 2.074(4) . ?
Pt1b N2b 2.185(4) . ?
Pt1b Cl1b 2.3050(12) . ?
C8b C7b 1.322(7) . ?
C7b C1b 1.481(7) . ?
C1b C6b 1.387(8) . ?
C1b C2b 1.397(7) . ?
C2b C3b 1.390(8) . ?
C3b C4b 1.375(9) . ?
C4b C5b 1.376(8) . ?
C5b C6b 1.398(7) . ?
N2b C13b 1.464(7) . ?
N2b C14b 1.470(7) . ?
N2b C12b 1.475(7) . ?
C12b C11b 1.449(9) . ?
C11b N1b 1.480(7) . ?
N1b C9b 1.449(6) . ?
N1b C10b 1.484(7) . ?
Pt1c C8c 1.977(4) . ?
Pt1c N1c 2.072(4) . ?
Pt1c N2c 2.180(4) . ?
Pt1c Cl1c 2.3015(11) . ?
C8c C7c 1.330(6) . ?
C7c C1c 1.475(6) . ?
C1c C2c 1.393(6) . ?
C1c C6c 1.401(7) . ?
C6c C5c 1.379(7) . ?
C5c C4c 1.380(7) . ?
C4c C3c 1.374(8) . ?
C3c C2c 1.401(7) . ?
N2c C13c 1.466(6) . ?
N2c C12c 1.481(6) . ?
N2c C14c 1.483(6) . ?
C12c C11c 1.509(7) . ?
C11c N1c 1.490(6) . ?
N1c C9c 1.480(6) . ?
N1c C10c 1.484(6) . ?
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
C8a Pt1a N1a 92.42(17) . . ?
C8a Pt1a N2a 176.72(16) . . ?
N1a Pt1a N2a 84.78(15) . . ?
C8a Pt1a Cl1a 90.40(13) . . ?
N1a Pt1a Cl1a 175.52(11) . . ?
N2a Pt1a Cl1a 92.49(10) . . ?
C7a C8a Pt1a 127.4(4) . . ?
C8a C7a C1a 127.5(5) . . ?
C6a C1a C2a 117.5(5) . . ?
C6a C1a C7a 123.9(5) . . ?
C2a C1a C7a 118.6(5) . . ?
C1a C2a C3a 121.3(5) . . ?
C4a C3a C2a 120.4(5) . . ?
C3a C4a C5a 118.4(5) . . ?
C4a C5a C6a 121.7(6) . . ?
C5a C6a C1a 120.8(5) . . ?
C13a N2a C14a 108.9(4) . . ?
C13a N2a C12a 111.5(4) . . ?
C14a N2a C12a 107.5(4) . . ?
C13a N2a Pt1a 111.1(3) . . ?
C14a N2a Pt1a 113.6(3) . . ?
C12a N2a Pt1a 104.2(3) . . ?
N2a C12a C11a 109.4(4) . . ?
N1a C11a C12a 110.8(4) . . ?
C10a N1a C9a 108.2(4) . . ?
C10a N1a C11a 108.0(4) . . ?
C9a N1a C11a 110.2(4) . . ?
C10a N1a Pt1a 112.1(3) . . ?
C9a N1a Pt1a 111.7(3) . . ?
C11a N1a Pt1a 106.4(3) . . ?
C8b Pt1b N1b 91.91(18) . . ?
C8b Pt1b N2b 175.0(2) . . ?
N1b Pt1b N2b 84.36(15) . . ?
C8b Pt1b Cl1b 92.15(15) . . ?
N1b Pt1b Cl1b 174.93(11) . . ?
N2b Pt1b Cl1b 91.76(12) . . ?
C7b C8b Pt1b 131.7(4) . . ?
C8b C7b C1b 124.4(5) . . ?
C6b C1b C2b 117.6(5) . . ?
C6b C1b C7b 123.4(5) . . ?
C2b C1b C7b 119.0(5) . . ?
C3b C2b C1b 120.8(5) . . ?
C4b C3b C2b 120.8(5) . . ?
C3b C4b C5b 119.3(5) . . ?
C4b C5b C6b 120.1(6) . . ?
C1b C6b C5b 121.4(5) . . ?
C13b N2b C14b 109.4(5) . . ?
C13b N2b C12b 109.8(4) . . ?
C14b N2b C12b 108.9(5) . . ?
C13b N2b Pt1b 113.6(4) . . ?
C14b N2b Pt1b 109.9(3) . . ?
C12b N2b Pt1b 105.0(3) . . ?
C11b C12b N2b 114.0(5) . . ?
C12b C11b N1b 114.0(6) . . ?
C9b N1b C11b 112.6(5) . . ?
C9b N1b C10b 105.7(5) . . ?
C11b N1b C10b 105.2(5) . . ?
C9b N1b Pt1b 111.3(3) . . ?
C11b N1b Pt1b 106.6(3) . . ?
C10b N1b Pt1b 115.3(3) . . ?
C8c Pt1c N1c 90.79(16) . . ?
C8c Pt1c N2c 175.27(16) . . ?
N1c Pt1c N2c 84.54(15) . . ?
C8c Pt1c Cl1c 91.71(13) . . ?
N1c Pt1c Cl1c 177.46(11) . . ?
N2c Pt1c Cl1c 92.96(11) . . ?
C7c C8c Pt1c 128.1(4) . . ?
C8c C7c C1c 127.1(4) . . ?
C2c C1c C6c 117.6(4) . . ?
C2c C1c C7c 120.3(4) . . ?
C6c C1c C7c 122.1(4) . . ?
C5c C6c C1c 120.6(5) . . ?
C6c C5c C4c 121.3(5) . . ?
C3c C4c C5c 119.1(5) . . ?
C4c C3c C2c 120.2(5) . . ?
C1c C2c C3c 121.0(5) . . ?
C13c N2c C12c 108.8(4) . . ?
C13c N2c C14c 109.1(4) . . ?
C12c N2c C14c 110.2(4) . . ?
C13c N2c Pt1c 113.8(3) . . ?
C12c N2c Pt1c 104.1(3) . . ?
C14c N2c Pt1c 110.7(3) . . ?
N2c C12c C11c 109.8(4) . . ?
N1c C11c C12c 110.5(4) . . ?
C9c N1c C10c 108.3(4) . . ?
C9c N1c C11c 109.7(4) . . ?
C10c N1c C11c 107.6(4) . . ?
C9c N1c Pt1c 110.8(3) . . ?
C10c N1c Pt1c 113.6(3) . . ?
C11c N1c Pt1c 106.7(3) . . ?
_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         3.182
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.159


data_Z2a
_database_code_depnum_ccdc_archive 'CCDC 904375'
#TrackingRef 'web_deposit_cif_file_0_ConcettaPacifico_1349943769.all.cif'
_audit_creation_date             05-08-16
_exptl_crystal_recrystallization_method 
;
>From hexane/CH2Cl2
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Pt(Me2NCH2CH2NMe2)(C8H7)Cl]'
_chemical_formula_sum            'C14 H23 Cl N2 Pt'
_chemical_formula_weight         449.88
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'
Cl Cl 0.1484 0.1585 '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'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a                   7.9854(4)
_cell_length_b                   20.2676(10)
_cell_length_c                   9.6517(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.931(3)
_cell_angle_gamma                90.00
_cell_volume                     1547.14(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7615
_cell_measurement_theta_min      2
_cell_measurement_theta_max      30.5
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.27
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             864
_exptl_absorpt_coefficient_mu    9.228
_exptl_absorpt_correction_type   Multiscan
_exptl_absorpt_correction_T_min  0.031
_exptl_absorpt_correction_T_max  0.080
_exptl_absorpt_process_details   Sadabs
_exptl_special_details           
;
Data collection optimised with COSMO.
Oxford Crysosystems LT device.
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'Omega and phi'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14968
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         30.48
_reflns_number_total             4319
_reflns_number_gt                3576
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       Smart
_computing_cell_refinement       Saint
_computing_data_reduction        Saint
_computing_structure_solution    Dirdif
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    XP
_computing_publication_material  'XCIF, PLATON'
_refine_special_details          
;
Lowish crystal quality; the crystal was rather an irregular shape.
The peak shapes were rather poor & broad.
761_ALERT_1_A CIF Contains no X-H Bonds ...................... ?
762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ?
No action taken.
911_ALERT_3_B # Missing FCF Refl. Between TH(Min) & STH/L=0.6 11
912_ALERT_3_B # Missing FCF Reflections Above STH/L=0.6 ...... 382
The data collection strategy used aimed to achieve a complete data set to
2\q = 54 deg. Some higher angle data were collected in the process and these
have been included in the refinement.
#===============================================================================
Resolution & Completeness Statistics (Cumulative)
#===============================================================================
Theta sin(th)/Lambda Complete Expected Measured Missing
#-------------------------------------------------------------------------------
20.82 0.500 0.996 1619 1613 6
23.01 0.550 0.995 2158 2148 10
25.24 0.600 0.996 2792 2781 11
#----------------------------------------------------------- ACTA Min. Res. ----
27.51 0.650 0.996 3575 3562 13
29.84 0.700 0.943 4455 4202 253
30.48 0.714 0.917 4712 4319 393
#===============================================================================
065_ALERT_3_A Crystal Requires Numerical Correction mu*tmid .. 4.06
060_ALERT_3_A Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 2.33
342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 13
Sadabs corrects for all systematic errors that lead to disparities in the
intensities of symmetry-equivalent data. These may include absorption by the
mount, crystal decay etc. Here the crystal quality was rather low; though
diffraction was strong the peak shapes were noticeable split. The crystal
was a rather irregular shape, and this precluded integration methods for
correcting for absorption.
042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C11
No action taken.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+12.1055P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geometric
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4319
_refine_ls_number_parameters     163
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0526
_refine_ls_wR_factor_ref         0.1313
_refine_ls_wR_factor_gt          0.1272
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_restrained_S_all      1.128
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
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 0.13583(4) 0.188612(13) 0.45174(3) 0.02377(11) Uani 1 1 d . . .
Cl1 Cl 0.3714(3) 0.24692(11) 0.4096(2) 0.0351(4) Uani 1 1 d . . .
C8 C 0.2734(12) 0.1073(4) 0.4766(9) 0.0357(18) Uani 1 1 d . . .
H8 H 0.3188 0.0988 0.5712 0.043 Uiso 1 1 calc R . .
C7 C 0.3155(11) 0.0617(4) 0.3868(9) 0.0337(17) Uani 1 1 d . . .
H7 H 0.3885 0.0278 0.4274 0.040 Uiso 1 1 calc R . .
C1 C 0.2647(10) 0.0564(4) 0.2333(9) 0.0298(16) Uani 1 1 d . . .
C2 C 0.1518(10) 0.0990(4) 0.1559(9) 0.0300(16) Uani 1 1 d . . .
H2 H 0.1059 0.1350 0.2012 0.036 Uiso 1 1 calc R . .
C3 C 0.1052(11) 0.0897(4) 0.0135(9) 0.0315(17) Uani 1 1 d . . .
H3 H 0.0266 0.1190 -0.0375 0.038 Uiso 1 1 calc R . .
C4 C 0.1732(13) 0.0377(5) -0.0555(10) 0.041(2) Uani 1 1 d . . .
H4 H 0.1407 0.0313 -0.1530 0.049 Uiso 1 1 calc R . .
C5 C 0.2875(14) -0.0042(5) 0.0188(11) 0.043(2) Uani 1 1 d . . .
H5 H 0.3355 -0.0392 -0.0279 0.052 Uiso 1 1 calc R . .
C6 C 0.3339(12) 0.0044(4) 0.1628(10) 0.0358(18) Uani 1 1 d . . .
H6 H 0.4125 -0.0249 0.2133 0.043 Uiso 1 1 calc R . .
N1 N -0.0829(9) 0.1423(3) 0.4946(7) 0.0287(14) Uani 1 1 d . . .
C11 C -0.2026(12) 0.1954(4) 0.5220(11) 0.0369(19) Uani 1 1 d . . .
H111 H -0.1737 0.2112 0.6195 0.044 Uiso 1 1 calc R . .
H112 H -0.3189 0.1774 0.5115 0.044 Uiso 1 1 calc R . .
C12 C -0.1964(11) 0.2523(4) 0.4235(10) 0.0355(18) Uani 1 1 d . . .
H121 H -0.2365 0.2380 0.3265 0.043 Uiso 1 1 calc R . .
H122 H -0.2711 0.2882 0.4479 0.043 Uiso 1 1 calc R . .
N2 N -0.0184(8) 0.2766(3) 0.4337(7) 0.0264(13) Uani 1 1 d . . .
C9 C -0.1614(12) 0.1008(5) 0.3757(10) 0.039(2) Uani 1 1 d . . .
H91 H -0.1812 0.1277 0.2907 0.059 Uiso 1 1 calc R . .
H92 H -0.2693 0.0832 0.3970 0.059 Uiso 1 1 calc R . .
H93 H -0.0854 0.0642 0.3613 0.059 Uiso 1 1 calc R . .
C10 C -0.0537(15) 0.0999(5) 0.6198(11) 0.048(2) Uani 1 1 d . . .
H101 H 0.0258 0.0647 0.6045 0.072 Uiso 1 1 calc R . .
H102 H -0.1611 0.0805 0.6375 0.072 Uiso 1 1 calc R . .
H103 H -0.0062 0.1264 0.7007 0.072 Uiso 1 1 calc R . .
C13 C -0.0043(13) 0.3170(4) 0.3065(10) 0.0370(19) Uani 1 1 d . . .
H131 H 0.1114 0.3338 0.3108 0.055 Uiso 1 1 calc R . .
H132 H -0.0834 0.3541 0.3023 0.055 Uiso 1 1 calc R . .
H133 H -0.0316 0.2895 0.2228 0.055 Uiso 1 1 calc R . .
C14 C 0.0271(12) 0.3195(4) 0.5587(10) 0.0348(18) Uani 1 1 d . . .
H141 H 0.1440 0.3347 0.5619 0.052 Uiso 1 1 calc R . .
H142 H 0.0161 0.2943 0.6437 0.052 Uiso 1 1 calc R . .
H143 H -0.0489 0.3577 0.5529 0.052 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.02498(16) 0.02584(15) 0.01965(16) -0.00048(10) 0.00012(10) 0.00000(10)
Cl1 0.0240(9) 0.0417(10) 0.0391(11) 0.0018(8) 0.0027(8) -0.0031(7)
C8 0.040(5) 0.037(4) 0.026(4) 0.005(3) -0.007(3) 0.002(4)
C7 0.034(4) 0.031(4) 0.034(4) 0.002(3) -0.004(3) 0.007(3)
C1 0.025(4) 0.030(4) 0.035(4) -0.002(3) 0.008(3) -0.002(3)
C2 0.031(4) 0.027(4) 0.032(4) 0.000(3) 0.005(3) 0.003(3)
C3 0.037(4) 0.030(4) 0.027(4) 0.000(3) 0.005(3) -0.004(3)
C4 0.055(6) 0.037(4) 0.029(5) -0.006(3) 0.007(4) -0.005(4)
C5 0.053(6) 0.033(4) 0.046(6) -0.006(4) 0.015(5) 0.003(4)
C6 0.038(5) 0.030(4) 0.041(5) 0.000(3) 0.011(4) 0.005(3)
N1 0.033(4) 0.030(3) 0.024(3) -0.001(3) 0.005(3) -0.002(3)
C11 0.030(4) 0.042(5) 0.040(5) -0.004(4) 0.011(4) -0.007(3)
C12 0.031(4) 0.036(4) 0.038(5) -0.004(4) -0.001(4) 0.000(3)
N2 0.025(3) 0.034(3) 0.018(3) 0.001(2) -0.004(2) 0.000(2)
C9 0.041(5) 0.040(5) 0.037(5) -0.009(4) 0.005(4) -0.011(4)
C10 0.058(7) 0.046(5) 0.039(5) 0.018(4) 0.003(5) -0.003(5)
C13 0.042(5) 0.042(5) 0.027(4) 0.007(3) 0.002(4) 0.005(4)
C14 0.037(5) 0.033(4) 0.034(5) -0.009(3) 0.002(4) 0.000(3)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Pt1 C8 1.977(9) . ?
Pt1 N1 2.074(7) . ?
Pt1 N2 2.161(7) . ?
Pt1 Cl1 2.305(2) . ?
C8 C7 1.341(12) . ?
C7 C1 1.485(12) . ?
C1 C2 1.389(11) . ?
C1 C6 1.407(11) . ?
C2 C3 1.386(12) . ?
C3 C4 1.397(13) . ?
C4 C5 1.374(14) . ?
C5 C6 1.399(14) . ?
N1 C10 1.475(11) . ?
N1 C11 1.488(11) . ?
N1 C9 1.489(11) . ?
C11 C12 1.499(13) . ?
C12 N2 1.495(11) . ?
N2 C14 1.491(10) . ?
N2 C13 1.492(11) . ?
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
C8 Pt1 N1 93.9(3) . . ?
C8 Pt1 N2 177.4(3) . . ?
N1 Pt1 N2 84.5(3) . . ?
C8 Pt1 Cl1 89.8(3) . . ?
N1 Pt1 Cl1 175.96(19) . . ?
N2 Pt1 Cl1 91.87(18) . . ?
C7 C8 Pt1 132.9(7) . . ?
C8 C7 C1 129.5(8) . . ?
C2 C1 C6 118.3(8) . . ?
C2 C1 C7 124.0(7) . . ?
C6 C1 C7 117.7(8) . . ?
C3 C2 C1 121.0(8) . . ?
C2 C3 C4 120.4(8) . . ?
C5 C4 C3 119.4(9) . . ?
C4 C5 C6 120.5(8) . . ?
C5 C6 C1 120.4(8) . . ?
C10 N1 C11 108.0(7) . . ?
C10 N1 C9 107.7(7) . . ?
C11 N1 C9 109.5(7) . . ?
C10 N1 Pt1 112.6(6) . . ?
C11 N1 Pt1 106.7(5) . . ?
C9 N1 Pt1 112.3(5) . . ?
N1 C11 C12 111.4(7) . . ?
N2 C12 C11 109.1(7) . . ?
C14 N2 C13 108.0(7) . . ?
C14 N2 C12 111.7(7) . . ?
C13 N2 C12 107.8(7) . . ?
C14 N2 Pt1 110.1(5) . . ?
C13 N2 Pt1 114.3(5) . . ?
C12 N2 Pt1 105.0(5) . . ?
_diffrn_measured_fraction_theta_max 0.917
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         4.704
_refine_diff_density_min         -3.491
_refine_diff_density_rms         0.288


data_E2b_II
_database_code_depnum_ccdc_archive 'CCDC 904377'
#TrackingRef 'web_deposit_cif_file_0_ConcettaPacifico_1349943769.all.cif'
_exptl_crystal_recrystallization_method 'Hexane diffused into DCM in freezer'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H25 Cl N2 O Pt'
_chemical_formula_sum            'C15 H25 Cl N2 O Pt'
_chemical_formula_weight         479.91
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_int_tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
_cell_length_a                   10.0881(6)
_cell_length_b                   12.1859(6)
_cell_length_c                   13.5748(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1668.79(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6034
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      28.5
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             928
_exptl_absorpt_coefficient_mu    8.566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.14
_exptl_absorpt_correction_T_max  0.28
_exptl_absorpt_process_details   'SABABS 2004/1'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       sphere
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19914
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         28.88
_reflns_number_total             4104
_reflns_number_gt                3923
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       SMART
_computing_cell_refinement       SAINT
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    XP
_computing_publication_material  'PLATON, ENCIFER, XCIF'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
>>> The Following ALERTS were generated <<<
#------------------------------------------
Format: alert-number_ALERT_alert-type_alert-level text
060_ALERT_3_A Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 3.26
Sadabs corrects for all systematic errors that lead to disparities in the
intensities of symmetry-equivalent data. These may include absorption by the
mount, crystal decay etc. The crystal was a rather irregular shape, this
precluded integration methods for correcting for absorption.
029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.96
912_ALERT_3_B # Missing FCF Reflections Above STH/L=0.6 ...... 106
See completeness statistics below
INTENSITY STATISTICS FOR DATASET # 1 ps0516.hkl
Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma)
Inf - 2.20 124 124 100.0 10.17 1497.5 49.64 0.0400 0.0194
2.20 - 1.65 138 138 100.0 12.11 1061.0 53.90 0.0389 0.0176
1.65 - 1.40 148 148 100.0 11.75 684.3 48.76 0.0450 0.0185
1.40 - 1.25 152 152 100.0 11.05 590.3 46.75 0.0434 0.0196
1.25 - 1.15 143 143 100.0 10.17 474.9 42.14 0.0504 0.0206
1.15 - 1.05 208 208 100.0 9.44 388.8 37.75 0.0492 0.0234
1.05 - 1.00 136 136 100.0 9.04 374.4 35.50 0.0507 0.0245
1.00 - 0.95 163 163 100.0 8.54 299.3 31.56 0.0538 0.0267
0.95 - 0.90 201 201 100.0 7.96 256.5 29.35 0.0525 0.0286
0.90 - 0.85 248 248 100.0 7.64 214.6 25.75 0.0607 0.0329
0.85 - 0.80 311 311 100.0 7.01 181.1 21.87 0.0649 0.0386
0.80 - 0.75 380 413 92.0 4.46 139.9 15.29 0.0701 0.0621
0.75 - 0.74 50 123 40.7 0.67 127.2 6.94 0.0733 0.1343
#-----------------------------------------------------------------------------
0.85 - 0.74 741 847 87.5 4.85 156.3 17.49 0.0671 0.0546
Inf - 0.74 2402 2508 95.8 7.97 413.1 32.06 0.0466 0.0254
Merged [A], lowest resolution = 13.57 Angstroms, 863 outliers downweighted
795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C1
No action taken
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0134P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(6)
_refine_ls_number_reflns         4104
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0177
_refine_ls_wR_factor_ref         0.0386
_refine_ls_wR_factor_gt          0.0384
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
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 0.101743(12) 0.186549(9) 0.112983(8) 0.01969(4) Uani 1 1 d . . .
Cl1 Cl 0.01596(9) 0.35772(7) 0.08007(6) 0.03002(18) Uani 1 1 d . . .
O1 O 0.1613(3) 0.3797(2) 0.71301(17) 0.0316(6) Uani 1 1 d . . .
N2 N 0.0773(3) 0.1356(2) -0.03981(18) 0.0263(6) Uani 1 1 d . . .
C9 C 0.3248(4) 0.0356(3) 0.1439(3) 0.0366(9) Uani 1 1 d . . .
H91 H 0.3473 0.0800 0.2017 0.055 Uiso 1 1 calc R . .
H92 H 0.3636 0.0690 0.0849 0.055 Uiso 1 1 calc R . .
H93 H 0.3599 -0.0388 0.1522 0.055 Uiso 1 1 calc R . .
C4 C 0.1833(3) 0.3525(2) 0.6153(2) 0.0248(6) Uani 1 1 d . . .
C8 C 0.1142(4) 0.2253(3) 0.2553(2) 0.0261(7) Uani 1 1 d . . .
H8 H 0.0342 0.2135 0.2907 0.031 Uiso 1 1 calc R . .
C3 C 0.2851(3) 0.3932(3) 0.5584(2) 0.0251(7) Uani 1 1 d . . .
H3 H 0.3490 0.4415 0.5860 0.030 Uiso 1 1 calc R . .
C1 C 0.2025(3) 0.2917(2) 0.4156(2) 0.0229(6) Uani 1 1 d . . .
C11 C 0.1368(4) -0.0348(3) 0.0452(3) 0.0393(10) Uani 1 1 d . . .
H111 H 0.1917 -0.1019 0.0407 0.047 Uiso 1 1 calc R . .
H112 H 0.0431 -0.0575 0.0529 0.047 Uiso 1 1 calc R . .
N1 N 0.1783(3) 0.0306(2) 0.13296(18) 0.0273(6) Uani 1 1 d . . .
C13 C 0.1344(4) 0.2118(3) -0.1131(2) 0.0354(8) Uani 1 1 d . . .
H131 H 0.2291 0.2219 -0.0997 0.053 Uiso 1 1 calc R . .
H132 H 0.0891 0.2828 -0.1088 0.053 Uiso 1 1 calc R . .
H133 H 0.1229 0.1814 -0.1793 0.053 Uiso 1 1 calc R . .
C6 C 0.1032(4) 0.2494(3) 0.4768(2) 0.0263(7) Uani 1 1 d . . .
H6 H 0.0417 0.1982 0.4505 0.032 Uiso 1 1 calc R . .
C10 C 0.1250(4) -0.0280(3) 0.2208(3) 0.0397(10) Uani 1 1 d . . .
H101 H 0.0281 -0.0308 0.2169 0.060 Uiso 1 1 calc R . .
H102 H 0.1514 0.0112 0.2807 0.060 Uiso 1 1 calc R . .
H103 H 0.1605 -0.1028 0.2226 0.060 Uiso 1 1 calc R . .
C15 C 0.2649(4) 0.4379(3) 0.7619(3) 0.0372(9) Uani 1 1 d . . .
H151 H 0.2387 0.4527 0.8302 0.056 Uiso 1 1 calc R . .
H152 H 0.2813 0.5075 0.7278 0.056 Uiso 1 1 calc R . .
H153 H 0.3460 0.3936 0.7614 0.056 Uiso 1 1 calc R . .
C7 C 0.2110(4) 0.2638(3) 0.3098(2) 0.0267(7) Uani 1 1 d . . .
H7 H 0.2941 0.2747 0.2784 0.032 Uiso 1 1 calc R . .
C5 C 0.0923(4) 0.2804(3) 0.5749(2) 0.0271(7) Uani 1 1 d . . .
H5 H 0.0223 0.2522 0.6143 0.033 Uiso 1 1 calc R . .
C14 C -0.0647(4) 0.1222(4) -0.0607(3) 0.0404(10) Uani 1 1 d . . .
H141 H -0.1094 0.1932 -0.0544 0.061 Uiso 1 1 calc R . .
H142 H -0.1032 0.0700 -0.0138 0.061 Uiso 1 1 calc R . .
H143 H -0.0761 0.0943 -0.1279 0.061 Uiso 1 1 calc R . .
C2 C 0.2928(3) 0.3623(3) 0.4594(2) 0.0251(7) Uani 1 1 d . . .
H2 H 0.3630 0.3909 0.4204 0.030 Uiso 1 1 calc R . .
C12 C 0.1515(4) 0.0301(3) -0.0466(3) 0.0393(10) Uani 1 1 d . . .
H121 H 0.1177 -0.0130 -0.1030 0.047 Uiso 1 1 calc R . .
H122 H 0.2466 0.0455 -0.0583 0.047 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.02269(6) 0.01932(5) 0.01707(5) -0.00041(5) 0.00019(5) -0.00194(5)
Cl1 0.0371(5) 0.0217(4) 0.0312(4) -0.0023(3) -0.0059(4) 0.0029(3)
O1 0.0400(15) 0.0342(13) 0.0205(11) -0.0045(10) 0.0002(11) -0.0049(11)
N2 0.0342(18) 0.0270(14) 0.0178(12) -0.0016(11) 0.0006(12) 0.0010(12)
C9 0.029(2) 0.034(2) 0.047(2) 0.0058(16) 0.0040(17) 0.0051(16)
C4 0.0308(17) 0.0239(14) 0.0197(13) 0.0007(13) -0.0043(16) 0.0062(13)
C8 0.0306(18) 0.0279(15) 0.0196(14) -0.0006(12) -0.0008(15) 0.0000(15)
C3 0.0233(17) 0.0248(16) 0.0272(16) -0.0002(13) -0.0050(14) -0.0009(13)
C1 0.0241(15) 0.0230(16) 0.0216(14) 0.0014(11) -0.0039(13) 0.0029(13)
C11 0.051(3) 0.0281(19) 0.039(2) -0.0051(15) 0.0022(17) 0.0025(17)
N1 0.0320(16) 0.0265(14) 0.0234(14) 0.0017(10) -0.0010(12) 0.0032(12)
C13 0.049(2) 0.0381(18) 0.0191(14) 0.0035(15) 0.0020(15) 0.0007(16)
C6 0.0282(16) 0.0247(15) 0.0259(15) -0.0012(12) -0.0041(15) -0.0011(16)
C10 0.041(2) 0.034(2) 0.044(2) 0.0166(16) 0.0059(18) 0.0013(17)
C15 0.046(2) 0.036(2) 0.0301(17) -0.0107(17) -0.0051(16) -0.0039(18)
C7 0.0266(18) 0.0277(16) 0.0258(16) 0.0027(13) 0.0039(14) 0.0009(15)
C5 0.0301(18) 0.0276(16) 0.0237(14) 0.0024(13) 0.0019(15) -0.0043(15)
C14 0.040(2) 0.051(2) 0.0301(18) -0.0072(17) -0.0067(17) -0.0114(18)
C2 0.0225(17) 0.0277(16) 0.0250(15) 0.0011(13) -0.0016(14) 0.0021(14)
C12 0.061(3) 0.0302(19) 0.0263(17) -0.0056(15) 0.0014(17) 0.0037(17)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Pt1 C8 1.992(3) . ?
Pt1 N1 2.069(3) . ?
Pt1 N2 2.179(3) . ?
Pt1 Cl1 2.3021(8) . ?
O1 C4 1.385(4) . ?
O1 C15 1.427(4) . ?
N2 C14 1.469(4) . ?
N2 C13 1.478(4) . ?
N2 C12 1.490(5) . ?
C9 N1 1.487(5) . ?
C9 H91 0.9800 . ?
C9 H92 0.9800 . ?
C9 H93 0.9800 . ?
C4 C3 1.377(5) . ?
C4 C5 1.384(5) . ?
C8 C7 1.312(5) . ?
C8 H8 0.9500 . ?
C3 C2 1.398(4) . ?
C3 H3 0.9500 . ?
C1 C2 1.387(4) . ?
C1 C6 1.399(5) . ?
C1 C7 1.479(4) . ?
C11 C12 1.483(6) . ?
C11 N1 1.493(4) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
N1 C10 1.490(4) . ?
C13 H131 0.9800 . ?
C13 H132 0.9800 . ?
C13 H133 0.9800 . ?
C6 C5 1.390(4) . ?
C6 H6 0.9500 . ?
C10 H101 0.9800 . ?
C10 H102 0.9800 . ?
C10 H103 0.9800 . ?
C15 H151 0.9800 . ?
C15 H152 0.9800 . ?
C15 H153 0.9800 . ?
C2 H200 0.9500 . ?
C5 H5 0.9500 . ?
C14 H141 0.9800 . ?
C14 H142 0.9800 . ?
C14 H143 0.9800 . ?
C2 H2 0.9500 . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
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
C8 Pt1 N1 93.84(11) . . ?
C8 Pt1 N2 175.89(13) . . ?
N1 Pt1 N2 84.55(10) . . ?
C8 Pt1 Cl1 89.84(10) . . ?
N1 Pt1 Cl1 176.31(7) . . ?
N2 Pt1 Cl1 91.78(7) . . ?
C4 O1 C15 116.6(3) . . ?
C14 N2 C13 108.6(3) . . ?
C14 N2 C12 112.4(3) . . ?
C13 N2 C12 107.8(3) . . ?
C14 N2 Pt1 109.0(2) . . ?
C13 N2 Pt1 114.7(2) . . ?
C12 N2 Pt1 104.34(19) . . ?
N1 C9 H91 109.5 . . ?
N1 C9 H92 109.5 . . ?
H91 C9 H92 109.5 . . ?
N1 C9 H93 109.5 . . ?
H91 C9 H93 109.5 . . ?
H92 C9 H93 109.5 . . ?
C3 C4 C5 120.1(3) . . ?
C3 C4 O1 124.8(3) . . ?
C5 C4 O1 115.1(3) . . ?
C7 C8 Pt1 132.7(3) . . ?
C7 C8 H8 113.6 . . ?
Pt1 C8 H8 113.6 . . ?
C4 C3 C2 119.0(3) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C2 C1 C6 116.4(3) . . ?
C2 C1 C7 121.4(3) . . ?
C6 C1 C7 122.2(3) . . ?
C12 C11 N1 111.0(3) . . ?
C12 C11 H111 109.4 . . ?
N1 C11 H111 109.4 . . ?
C12 C11 H112 109.4 . . ?
N1 C11 H112 109.4 . . ?
H111 C11 H112 108.0 . . ?
C9 N1 C10 107.4(3) . . ?
C9 N1 C11 112.4(3) . . ?
C10 N1 C11 106.4(3) . . ?
C9 N1 Pt1 110.2(2) . . ?
C10 N1 Pt1 114.2(2) . . ?
C11 N1 Pt1 106.3(2) . . ?
N2 C13 H131 109.5 . . ?
N2 C13 H132 109.5 . . ?
H131 C13 H132 109.5 . . ?
N2 C13 H133 109.5 . . ?
H131 C13 H133 109.5 . . ?
H132 C13 H133 109.5 . . ?
C5 C6 C1 121.7(3) . . ?
C5 C6 H6 119.1 . . ?
C1 C6 H6 119.1 . . ?
N1 C10 H101 109.5 . . ?
N1 C10 H102 109.5 . . ?
H101 C10 H102 109.5 . . ?
N1 C10 H103 109.5 . . ?
H101 C10 H103 109.5 . . ?
H102 C10 H103 109.5 . . ?
O1 C15 H151 109.5 . . ?
O1 C15 H152 109.5 . . ?
H151 C15 H152 109.5 . . ?
O1 C15 H153 109.5 . . ?
H151 C15 H153 109.5 . . ?
H152 C15 H153 109.5 . . ?
C8 C7 C1 125.9(3) . . ?
C8 C7 H7 117.0 . . ?
C1 C7 H7 117.0 . . ?
C4 C5 C6 120.0(3) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
N2 C14 H141 109.5 . . ?
N2 C14 H142 109.5 . . ?
H141 C14 H142 109.5 . . ?
N2 C14 H43 109.5 . . ?
H141 C14 H142 109.5 . . ?
H142 C14 H143 109.5 . . ?
C1 C2 C3 122.8(3) . . ?
C1 C2 H2 118.6 . . ?
C3 C2 H2 118.6 . . ?
C11 C12 N2 111.0(3) . . ?
C11 C12 H121 109.4 . . ?
N2 C12 H121 109.4 . . ?
C11 C12 H122 109.4 . . ?
N2 C12 H122 109.4 . . ?
H121 C12 H122 108.0 . . ?
_diffrn_measured_fraction_theta_max 0.957
_diffrn_reflns_theta_full        28.88
_diffrn_measured_fraction_theta_full 0.957
_refine_diff_density_max         1.350
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.097


data_E2c
_database_code_depnum_ccdc_archive 'CCDC 904378'
#TrackingRef 'web_deposit_cif_file_0_ConcettaPacifico_1357638037.carmen.cif'
_audit_update_record             
;
2012-09-11 # Formatted by publCIF
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H22 Cl N3 O2 Pt'
_chemical_formula_sum            'C14 H22 Cl N3 O2 Pt'
_chemical_formula_weight         494.88
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a                   27.2807(7)
_cell_length_b                   8.1215(2)
_cell_length_c                   15.6844(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.4263(19)
_cell_angle_gamma                90.00
_cell_volume                     3445.89(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5303
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      28.36
_exptl_crystal_description       tabular
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.026
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1904
_exptl_absorpt_coefficient_mu    8.306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7209
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   '(SADABS; G. M. Sheldrick, 1996)'
_exptl_special_details           ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BrukerAXS X8 APEX CCD system'
_diffrn_measurement_method       '\f and \w'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32586
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.62
_diffrn_reflns_theta_max         28.36
_reflns_number_total             4290
_reflns_number_gt                3364
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'SAINT-IRIX package'
_computing_cell_refinement       'SAINT-IRIX package'
_computing_data_reduction        'SAINT-IRIX package'
_computing_structure_solution    'SIR2004 (Burla, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury, Ortep for Window'
_computing_publication_material  'WinGX, PARST97'
_refine_special_details          
;
?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0857P)^2^+20.2848P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4290
_refine_ls_number_parameters     194
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0473
_refine_ls_wR_factor_ref         0.1364
_refine_ls_wR_factor_gt          0.1231
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
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 0.162644(10) 0.21027(3) 0.784925(18) 0.03824(12) Uani 1 1 d . . .
Cl1 Cl 0.20065(9) 0.4322(3) 0.85731(16) 0.0580(5) Uani 1 1 d . . .
N1 N 0.1310(3) 0.0011(9) 0.7256(5) 0.0503(16) Uani 1 1 d . . .
N2 N 0.2084(2) 0.0357(8) 0.8629(5) 0.0446(15) Uani 1 1 d . . .
C8 C 0.1185(3) 0.3648(11) 0.7127(6) 0.0498(19) Uani 1 1 d . . .
H8 H 0.0944 0.4158 0.7405 0.060 Uiso 1 1 calc R . .
C11 C 0.1471(4) -0.1421(12) 0.7805(6) 0.062(2) Uani 1 1 d . . .
H111 H 0.1422 -0.2428 0.7473 0.074 Uiso 1 1 calc R . .
H112 H 0.1276 -0.1488 0.8279 0.074 Uiso 1 1 calc R . .
C12 C 0.2013(4) -0.1230(10) 0.8150(7) 0.061(2) Uani 1 1 d . . .
H121 H 0.2119 -0.2140 0.8530 0.074 Uiso 1 1 calc R . .
H122 H 0.2211 -0.1236 0.7679 0.074 Uiso 1 1 calc R . .
C13 C 0.2625(3) 0.0718(14) 0.8737(8) 0.067(3) Uani 1 1 d . . .
H131 H 0.2802 -0.0181 0.9031 0.100 Uiso 1 1 calc R . .
H132 H 0.2689 0.1708 0.9067 0.100 Uiso 1 1 calc R . .
H133 H 0.2733 0.0860 0.8182 0.100 Uiso 1 1 calc R . .
C14 C 0.1925(4) 0.0228(14) 0.9494(7) 0.067(3) Uani 1 1 d . . .
H141 H 0.1970 0.1271 0.9782 0.100 Uiso 1 1 calc R . .
H142 H 0.2120 -0.0595 0.9822 0.100 Uiso 1 1 calc R . .
H143 H 0.1582 -0.0076 0.9440 0.100 Uiso 1 1 calc R . .
C9 C 0.1464(5) -0.0185(14) 0.6382(7) 0.080(3) Uani 1 1 d . . .
H91 H 0.1308 0.0649 0.6007 0.119 Uiso 1 1 calc R . .
H92 H 0.1365 -0.1253 0.6159 0.119 Uiso 1 1 calc R . .
H93 H 0.1816 -0.0079 0.6419 0.119 Uiso 1 1 calc R . .
C10 C 0.0764(4) 0.0047(14) 0.7163(9) 0.076(3) Uani 1 1 d . . .
H101 H 0.0635 -0.0959 0.6902 0.113 Uiso 1 1 calc R . .
H102 H 0.0645 0.0962 0.6807 0.113 Uiso 1 1 calc R . .
H103 H 0.0657 0.0162 0.7719 0.113 Uiso 1 1 calc R . .
C7 C 0.1182(3) 0.4060(11) 0.6308(6) 0.051(2) Uani 1 1 d . . .
H7 H 0.1414 0.3543 0.6015 0.061 Uiso 1 1 calc R . .
C1 C 0.0852(3) 0.5241(10) 0.5816(6) 0.0492(19) Uani 1 1 d . . .
C2 C 0.0418(3) 0.5840(10) 0.6075(6) 0.0488(19) Uani 1 1 d . . .
H2 H 0.0321 0.5488 0.6592 0.059 Uiso 1 1 calc R . .
C3 C 0.0132(4) 0.6944(10) 0.5576(7) 0.055(2) Uani 1 1 d . . .
C4 C 0.0252(4) 0.7533(14) 0.4810(8) 0.068(3) Uani 1 1 d . . .
H4 H 0.0053 0.8290 0.4483 0.081 Uiso 1 1 calc R . .
C5 C 0.0689(5) 0.6945(14) 0.4544(8) 0.073(3) Uani 1 1 d . . .
H5 H 0.0785 0.7321 0.4031 0.088 Uiso 1 1 calc R . .
C6 C 0.0979(4) 0.5817(14) 0.5030(7) 0.063(2) Uani 1 1 d . . .
H6 H 0.1265 0.5427 0.4834 0.075 Uiso 1 1 calc R . .
N3 N -0.0328(4) 0.7523(13) 0.5884(9) 0.079(3) Uani 1 1 d . . .
O1 O -0.0427(4) 0.6940(15) 0.6566(8) 0.110(4) Uani 1 1 d . . .
O2 O -0.0587(4) 0.8491(13) 0.5435(9) 0.115(4) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.04297(19) 0.03427(17) 0.03700(18) -0.00184(11) 0.00329(11) -0.00197(11)
Cl1 0.0654(13) 0.0424(10) 0.0638(14) -0.0098(9) -0.0009(10) -0.0089(9)
N1 0.056(4) 0.044(3) 0.049(4) -0.004(3) -0.001(3) -0.007(3)
N2 0.042(3) 0.042(3) 0.049(4) -0.005(3) 0.002(3) 0.006(3)
C8 0.050(5) 0.048(4) 0.050(5) -0.002(4) 0.001(4) 0.005(4)
C11 0.081(6) 0.044(5) 0.058(6) -0.004(4) 0.002(5) -0.014(5)
C12 0.074(6) 0.032(4) 0.078(7) -0.002(4) 0.010(5) 0.004(4)
C13 0.045(5) 0.065(6) 0.090(8) 0.002(6) 0.002(5) 0.006(4)
C14 0.074(6) 0.074(7) 0.053(6) 0.011(5) 0.010(5) 0.006(5)
C9 0.129(10) 0.058(6) 0.050(6) -0.018(5) 0.006(6) -0.007(6)
C10 0.065(6) 0.065(6) 0.091(8) -0.011(6) -0.014(5) -0.019(5)
C7 0.036(4) 0.058(5) 0.059(5) 0.001(4) 0.003(4) -0.002(3)
C1 0.041(4) 0.043(4) 0.061(5) -0.001(4) -0.004(4) -0.007(3)
C2 0.048(4) 0.043(4) 0.054(5) -0.007(4) 0.001(4) -0.006(3)
C3 0.049(5) 0.042(4) 0.070(6) -0.009(4) -0.010(4) 0.000(3)
C4 0.062(6) 0.056(5) 0.079(8) 0.006(5) -0.013(5) -0.006(5)
C5 0.080(8) 0.080(7) 0.054(6) 0.019(5) -0.008(5) -0.023(6)
C6 0.055(5) 0.074(6) 0.058(6) 0.006(5) 0.003(4) -0.013(5)
N3 0.060(6) 0.067(5) 0.109(9) -0.019(6) 0.004(6) 0.015(5)
O1 0.098(7) 0.137(10) 0.096(8) -0.007(7) 0.021(6) 0.056(6)
O2 0.082(6) 0.090(6) 0.167(11) 0.019(7) -0.007(6) 0.039(6)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Pt1 C8 1.990(9) . ?
Pt1 N1 2.071(7) . ?
Pt1 N2 2.160(7) . ?
Pt1 Cl1 2.304(2) . ?
N1 C11 1.480(12) . ?
N1 C10 1.479(13) . ?
N1 C9 1.492(13) . ?
N2 C14 1.480(12) . ?
N2 C13 1.495(11) . ?
N2 C12 1.492(11) . ?
C8 C7 1.326(13) . ?
C11 C12 1.515(15) . ?
C7 C1 1.465(12) . ?
C1 C2 1.389(12) . ?
C1 C6 1.404(13) . ?
C2 C3 1.366(13) . ?
C3 C4 1.372(17) . ?
C3 N3 1.478(15) . ?
C4 C5 1.397(18) . ?
C5 C6 1.375(16) . ?
N3 O2 1.219(15) . ?
N3 O1 1.231(16) . ?
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
C8 Pt1 N1 94.3(3) . . ?
C8 Pt1 N2 177.8(3) . . ?
N1 Pt1 N2 83.8(3) . . ?
C8 Pt1 Cl1 89.3(3) . . ?
N1 Pt1 Cl1 176.3(2) . . ?
N2 Pt1 Cl1 92.53(19) . . ?
C11 N1 C10 107.0(8) . . ?
C11 N1 C9 110.7(8) . . ?
C10 N1 C9 108.1(9) . . ?
C11 N1 Pt1 107.9(5) . . ?
C10 N1 Pt1 112.6(6) . . ?
C9 N1 Pt1 110.5(6) . . ?
C14 N2 C13 108.2(8) . . ?
C14 N2 C12 111.5(8) . . ?
C13 N2 C12 106.7(7) . . ?
C14 N2 Pt1 110.5(6) . . ?
C13 N2 Pt1 115.2(6) . . ?
C12 N2 Pt1 104.8(5) . . ?
C7 C8 Pt1 129.6(7) . . ?
N1 C11 C12 109.3(8) . . ?
N2 C12 C11 108.9(8) . . ?
C8 C7 C1 127.0(9) . . ?
C2 C1 C6 117.2(9) . . ?
C2 C1 C7 124.4(9) . . ?
C6 C1 C7 118.5(9) . . ?
C3 C2 C1 120.6(9) . . ?
C2 C3 C4 123.0(10) . . ?
C2 C3 N3 117.9(11) . . ?
C4 C3 N3 119.0(10) . . ?
C3 C4 C5 117.0(10) . . ?
C6 C5 C4 120.9(11) . . ?
C5 C6 C1 121.3(11) . . ?
O2 N3 O1 125.1(12) . . ?
O2 N3 C3 118.0(13) . . ?
O1 N3 C3 116.9(10) . . ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        28.36
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         7.764
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.213