#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/86/2018607.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2018607
loop_
_publ_author_name
'Giardina-Papa, Daniela'
'Intini, Francesco Paolo'
'Natile, Giovanni'
'Pacifico, Concetta'
_publ_section_title
;
 trans-Chloridobis[(Z)-1-imino-1-methoxyethane-κN](triphenylphosphane-κP)platinum(II)
 chloride monohydrate
;
_journal_coeditor_code           EG3099
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m300
_journal_page_last               m302
_journal_paper_doi               10.1107/S0108270112040826
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Pt Cl (C3 H7 N O)2 (C18 H15 P)] Cl, H2 O'
_chemical_formula_moiety         'C24 H29 Cl N2 O2 P Pt +, Cl -, H2 O'
_chemical_formula_sum            'C24 H31 Cl2 N2 O3 P Pt'
_chemical_formula_weight         692.47
_chemical_name_common
;
trans-[PtCl{E-HN=C(Me)OMe}₂(PPh₃)]Cl
;
_chemical_name_systematic
;
trans-Chloridobis[(Z)-1-imino-1-methoxyethane-
κN](triphenylphosphane-κP)platinum(II) chloride monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.0087(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7361(2)
_cell_length_b                   17.1215(2)
_cell_length_c                   15.6226(2)
_cell_measurement_reflns_used    30501
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      1.81
_cell_volume                     2731.03(7)
_computing_cell_refinement       'SAINT-IRIX (Bruker, 2004)'
_computing_data_collection
;
COSMO, APEX2 and BIS (Bruker, 2004)
;
_computing_data_reduction        'SAINT-IRIX (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
PARST97 (Nardelli, 1983, 1995) and WinGX (Farrugia,
1999)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30501
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.81
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.419
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.8888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.580
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         8334
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0358
_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)+(0.0214P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0648
_reflns_number_gt                5675
_reflns_number_total             8334
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            eg3099.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2018607
_cod_database_fobs_code          2018607
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Pt Pt1 0.474780(15) 0.639305(8) 0.262503(10) 0.02790(5) Uani d . 1 1
Cl Cl1 0.66397(11) 0.66329(6) 0.38493(8) 0.0494(3) Uani d D 1 1
N N1 0.5383(4) 0.72129(19) 0.1938(2) 0.0358(8) Uani d . 1 1
H H1 0.495(4) 0.763(2) 0.182(3) 0.043 Uiso d . 1 1
N N2 0.4236(4) 0.55760(17) 0.3381(2) 0.0335(8) Uani d . 1 1
H H2 0.475(4) 0.517(2) 0.354(3) 0.040 Uiso d . 1 1
P P1 0.29706(10) 0.61815(5) 0.14464(7) 0.0286(2) Uani d . 1 1
C C1 0.6304(5) 0.7141(2) 0.1593(3) 0.0443(11) Uani d . 1 1
C C2 0.6756(5) 0.7779(3) 0.1119(3) 0.0638(15) Uani d . 1 1
H H2A 0.6203 0.8227 0.1076 0.096 Uiso calc R 1 1
H H2B 0.6716 0.7608 0.0526 0.096 Uiso calc R 1 1
H H2C 0.7642 0.7915 0.1449 0.096 Uiso calc R 1 1
C C3 0.8019(7) 0.6321(3) 0.1438(6) 0.121(3) Uani d . 1 1
H H3A 0.7825 0.6425 0.0806 0.182 Uiso calc R 1 1
H H3B 0.8308 0.5790 0.1560 0.182 Uiso calc R 1 1
H H3C 0.8697 0.6668 0.1773 0.182 Uiso calc R 1 1
C C4 0.3323(5) 0.5578(2) 0.3742(3) 0.0378(10) Uani d . 1 1
C C5 0.3099(5) 0.4923(2) 0.4299(3) 0.0539(13) Uani d . 1 1
H H5A 0.3752 0.4528 0.4349 0.081 Uiso calc R 1 1
H H5B 0.2246 0.4704 0.4020 0.081 Uiso calc R 1 1
H H5C 0.3154 0.5112 0.4888 0.081 Uiso calc R 1 1
C C6 0.1477(6) 0.6250(3) 0.3957(5) 0.084(2) Uani d . 1 1
H H6A 0.0870 0.5830 0.3740 0.126 Uiso calc R 1 1
H H6B 0.1033 0.6740 0.3792 0.126 Uiso calc R 1 1
H H6C 0.1831 0.6219 0.4601 0.126 Uiso calc R 1 1
O O1 0.6863(3) 0.64405(18) 0.1698(3) 0.0639(10) Uani d . 1 1
O O2 0.2535(3) 0.61922(16) 0.3561(2) 0.0535(9) Uani d . 1 1
C C7 0.2200(4) 0.5243(2) 0.1507(3) 0.0332(9) Uani d . 1 1
C C8 0.2947(4) 0.4569(2) 0.1648(3) 0.0425(11) Uani d . 1 1
H H8 0.3832 0.4601 0.1699 0.051 Uiso calc R 1 1
C C9 0.2405(6) 0.3853(2) 0.1713(3) 0.0544(14) Uani d . 1 1
H H9 0.2905 0.3401 0.1770 0.065 Uiso calc R 1 1
C C10 0.1126(6) 0.3812(3) 0.1692(4) 0.0646(16) Uani d . 1 1
H H10 0.0767 0.3330 0.1756 0.078 Uiso calc R 1 1
C C11 0.0367(5) 0.4464(3) 0.1580(4) 0.0699(17) Uani d . 1 1
H H11 -0.0502 0.4429 0.1570 0.084 Uiso calc R 1 1
C C12 0.0913(5) 0.5187(3) 0.1480(3) 0.0534(13) Uani d . 1 1
H H12 0.0399 0.5635 0.1395 0.064 Uiso calc R 1 1
C C13 0.3298(4) 0.6192(2) 0.0372(3) 0.0323(9) Uani d . 1 1
C C14 0.3523(5) 0.6919(2) 0.0027(3) 0.0441(11) Uani d . 1 1
H H14 0.3439 0.7375 0.0328 0.053 Uiso calc R 1 1
C C15 0.3868(5) 0.6964(3) -0.0754(3) 0.0540(13) Uani d . 1 1
H H15 0.4043 0.7448 -0.0962 0.065 Uiso calc R 1 1
C C16 0.3953(5) 0.6297(3) -0.1223(3) 0.0597(14) Uani d . 1 1
H H16 0.4172 0.6329 -0.1753 0.072 Uiso calc R 1 1
C C17 0.3711(5) 0.5583(3) -0.0906(3) 0.0538(13) Uani d . 1 1
H H17 0.3749 0.5133 -0.1230 0.065 Uiso calc R 1 1
C C18 0.3410(5) 0.5528(2) -0.0102(3) 0.0439(11) Uani d . 1 1
H H18 0.3283 0.5039 0.0117 0.053 Uiso calc R 1 1
C C19 0.1728(4) 0.6935(2) 0.1282(3) 0.0325(9) Uani d . 1 1
C C20 0.1858(4) 0.7513(2) 0.1925(3) 0.0433(11) Uani d . 1 1
H H20 0.2524 0.7488 0.2471 0.052 Uiso calc R 1 1
C C21 0.0974(5) 0.8131(3) 0.1738(4) 0.0651(16) Uani d . 1 1
H H21 0.1056 0.8521 0.2166 0.078 Uiso calc R 1 1
C C22 -0.0006(5) 0.8179(3) 0.0945(4) 0.0653(17) Uani d . 1 1
H H22 -0.0574 0.8603 0.0828 0.078 Uiso calc R 1 1
C C23 -0.0154(5) 0.7600(3) 0.0318(4) 0.0628(15) Uani d . 1 1
H H23 -0.0838 0.7625 -0.0219 0.075 Uiso calc R 1 1
C C24 0.0713(4) 0.6976(3) 0.0481(3) 0.0495(12) Uani d . 1 1
H H24 0.0611 0.6584 0.0052 0.059 Uiso calc R 1 1
Cl Cl2 0.59138(13) 0.39386(6) 0.35942(9) 0.0528(3) Uani d D 1 1
O O1W 0.8280(6) 0.5086(3) 0.3327(5) 0.151(3) Uani d D 1 1
H H1W 0.795(6) 0.556(3) 0.350(6) 0.182 Uiso d D 1 1
H H2W 0.774(5) 0.473(4) 0.347(5) 0.182 Uiso d D 1 1
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'
P P 0.1023 0.0942 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N1 Pt1 N2 175.94(14) ?
N1 Pt1 P1 90.99(10) y
N2 Pt1 P1 93.01(10) y
N1 Pt1 Cl1 87.84(10) y
N2 Pt1 Cl1 88.16(10) y
P1 Pt1 Cl1 178.81(4) ?
C1 N1 Pt1 126.6(3) ?
C1 N1 H1 116(3) ?
Pt1 N1 H1 117(3) ?
C4 N2 Pt1 130.2(3) ?
C4 N2 H2 113(3) ?
Pt1 N2 H2 117(3) ?
C19 P1 C13 101.86(18) ?
C19 P1 C7 107.93(18) ?
C13 P1 C7 106.09(18) ?
C19 P1 Pt1 113.85(13) ?
C13 P1 Pt1 113.57(14) ?
C7 P1 Pt1 112.69(13) ?
N1 C1 O1 114.6(4) ?
N1 C1 C2 123.9(4) ?
O1 C1 C2 121.4(4) ?
C1 C2 H2A 109.5 ?
C1 C2 H2B 109.5 ?
H2A C2 H2B 109.5 ?
C1 C2 H2C 109.5 ?
H2A C2 H2C 109.5 ?
H2B C2 H2C 109.5 ?
O1 C3 H3A 109.5 ?
O1 C3 H3B 109.5 ?
H3A C3 H3B 109.5 ?
O1 C3 H3C 109.5 ?
H3A C3 H3C 109.5 ?
H3B C3 H3C 109.5 ?
N2 C4 O2 115.9(4) ?
N2 C4 C5 122.9(4) ?
O2 C4 C5 121.1(4) ?
C4 C5 H5A 109.5 ?
C4 C5 H5B 109.5 ?
H5A C5 H5B 109.5 ?
C4 C5 H5C 109.5 ?
H5A C5 H5C 109.5 ?
H5B C5 H5C 109.5 ?
O2 C6 H6A 109.5 ?
O2 C6 H6B 109.5 ?
H6A C6 H6B 109.5 ?
O2 C6 H6C 109.5 ?
H6A C6 H6C 109.5 ?
H6B C6 H6C 109.5 ?
C1 O1 C3 119.4(4) ?
C4 O2 C6 119.7(4) ?
C12 C7 C8 118.4(4) ?
C12 C7 P1 121.9(3) ?
C8 C7 P1 119.5(3) ?
C9 C8 C7 121.2(4) ?
C9 C8 H8 119.4 ?
C7 C8 H8 119.4 ?
C10 C9 C8 119.3(4) ?
C10 C9 H9 120.3 ?
C8 C9 H9 120.3 ?
C11 C10 C9 121.2(4) ?
C11 C10 H10 119.4 ?
C9 C10 H10 119.4 ?
C10 C11 C12 119.0(5) ?
C10 C11 H11 120.5 ?
C12 C11 H11 120.5 ?
C7 C12 C11 120.7(4) ?
C7 C12 H12 119.6 ?
C11 C12 H12 119.6 ?
C18 C13 C14 118.0(4) ?
C18 C13 P1 124.0(3) ?
C14 C13 P1 117.9(3) ?
C15 C14 C13 120.8(4) ?
C15 C14 H14 119.6 ?
C13 C14 H14 119.6 ?
C16 C15 C14 120.3(4) ?
C16 C15 H15 119.9 ?
C14 C15 H15 119.9 ?
C17 C16 C15 119.7(5) ?
C17 C16 H16 120.2 ?
C15 C16 H16 120.2 ?
C16 C17 C18 120.6(4) ?
C16 C17 H17 119.7 ?
C18 C17 H17 119.7 ?
C13 C18 C17 120.6(4) ?
C13 C18 H18 119.7 ?
C17 C18 H18 119.7 ?
C24 C19 C20 119.6(4) ?
C24 C19 P1 120.2(3) ?
C20 C19 P1 120.0(3) ?
C19 C20 C21 118.8(5) ?
C19 C20 H20 120.6 ?
C21 C20 H20 120.6 ?
C22 C21 C20 121.6(5) ?
C22 C21 H21 119.2 ?
C20 C21 H21 119.2 ?
C21 C22 C23 119.7(5) ?
C21 C22 H22 120.1 ?
C23 C22 H22 120.1 ?
C22 C23 C24 120.2(5) ?
C22 C23 H23 119.9 ?
C24 C23 H23 119.9 ?
C19 C24 C23 120.0(5) ?
C19 C24 H24 120.0 ?
C23 C24 H24 120.0 ?
H1W O1W H2W 100(7) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pt1 N1 2.010(3) y
Pt1 N2 2.014(3) y
Pt1 P1 2.2338(11) y
Pt1 Cl1 2.3559(11) y
N1 C1 1.270(5) ?
N1 H1 0.85(4) ?
N2 C4 1.273(5) ?
N2 H2 0.87(4) ?
P1 C19 1.816(4) ?
P1 C13 1.819(4) ?
P1 C7 1.823(4) ?
C1 O1 1.328(5) ?
C1 C2 1.484(6) ?
C2 H2A 0.96 ?
C2 H2B 0.96 ?
C2 H2C 0.96 ?
C3 O1 1.435(6) ?
C3 H3A 0.96 ?
C3 H3B 0.96 ?
C3 H3C 0.96 ?
C4 O2 1.324(5) ?
C4 C5 1.485(5) ?
C5 H5A 0.96 ?
C5 H5B 0.96 ?
C5 H5C 0.96 ?
C6 O2 1.455(6) ?
C6 H6A 0.96 ?
C6 H6B 0.96 ?
C6 H6C 0.96 ?
C7 C12 1.372(6) ?
C7 C8 1.384(5) ?
C8 C9 1.373(6) ?
C8 H8 0.93 ?
C9 C10 1.366(7) ?
C9 H9 0.93 ?
C10 C11 1.361(7) ?
C10 H10 0.93 ?
C11 C12 1.399(6) ?
C11 H11 0.93 ?
C12 H12 0.93 ?
C13 C18 1.382(5) ?
C13 C14 1.407(5) ?
C14 C15 1.381(6) ?
C14 H14 0.93 ?
C15 C16 1.376(6) ?
C15 H15 0.93 ?
C16 C17 1.374(6) ?
C16 H16 0.93 ?
C17 C18 1.393(6) ?
C17 H17 0.93 ?
C18 H18 0.93 ?
C19 C24 1.384(6) ?
C19 C20 1.386(5) ?
C20 C21 1.391(6) ?
C20 H20 0.93 ?
C21 C22 1.357(7) ?
C21 H21 0.93 ?
C22 C23 1.367(7) ?
C22 H22 0.93 ?
C23 C24 1.389(6) ?
C23 H23 0.93 ?
C24 H24 0.93 ?
O1W H1W 0.953(16) ?
O1W H2W 0.921(16) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1W H2W Cl2 . 0.921(16) 2.435(16) 3.337(5) 167(6)
N2 H2 Cl2 . 0.87(4) 2.45(4) 3.293(3) 166(4)
N1 H1 Cl2 2_655 0.85(4) 2.43(4) 3.262(4) 168(4)
C2 H2A Cl2 2_655 0.96 2.76 3.627(5) 149.9
C5 H5C Cl2 3_666 0.96 2.79 3.688(5) 155.5
C16 H16 Cl2 3_665 0.93 2.89 3.772(5) 159.9
O1W H1W Cl1 . 0.953(16) 2.477(16) 3.416(5) 168(6)
