#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:20:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179323 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/20/4322018.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_4322018
loop_
_publ_author_name
'Donald J. Darensbourg'
'Jeffrey B. Robertson'
'David L. Larkins'
'Joseph H. Reibenspies'
_publ_section_title
;
 Water-Soluble Organometallic Compounds. 7.1 Further Studies of
 1,3,5-Triaza-7-Phosphaadamantane Derivatives of Group 10 Metals,
 Including Metal Carbonyls and Hydrides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2473
_journal_page_last               2481
_journal_paper_doi               10.1021/ic981243j
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C24 H60 Cl N12 O6 P4 Pt'
_chemical_formula_weight         967.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           203
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 2uv 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.8476(19)
_cell_length_b                   19.8476(19)
_cell_length_c                   19.8476(19)
_cell_measurement_temperature    193(2)
_cell_volume                     7818.5(13)
_computing_cell_refinement       'XSCANS (SIEMENS, 1995)'
_computing_data_collection       'XSCANS (SIEMENS, 1995)'
_computing_molecular_graphics    'XP (SIEMENS, 1990)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.634
_diffrn_measured_fraction_theta_max 0.634
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       2
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            372
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.90
_diffrn_standards_decay_%        <1
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.874
_exptl_absorpt_correction_type   difabs
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3928
_refine_diff_density_max         1.391
_refine_diff_density_min         -1.612
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.00003(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0170P)²+500.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                294
_reflns_number_total             372
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic981243j_3.cif
_cod_data_source_block           dd385
_cod_original_sg_symbol_H-M      'F d -3'
_cod_database_code               4322018
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'-x+1/4, y, -z+1/4'
'x, -y+1/4, -z+1/4'
'z, x, y'
'z, -x+1/4, -y+1/4'
'-z+1/4, -x+1/4, y'
'-z+1/4, x, -y+1/4'
'y, z, x'
'-y+1/4, z, -x+1/4'
'y, -z+1/4, -x+1/4'
'-y+1/4, -z+1/4, x'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'-x+1/4, y+1/2, -z+3/4'
'x, -y+3/4, -z+3/4'
'z, x+1/2, y+1/2'
'z, -x+3/4, -y+3/4'
'-z+1/4, -x+3/4, y+1/2'
'-z+1/4, x+1/2, -y+3/4'
'y, z+1/2, x+1/2'
'-y+1/4, z+1/2, -x+3/4'
'y, -z+3/4, -x+3/4'
'-y+1/4, -z+3/4, x+1/2'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'-x+3/4, y, -z+3/4'
'x+1/2, -y+1/4, -z+3/4'
'z+1/2, x, y+1/2'
'z+1/2, -x+1/4, -y+3/4'
'-z+3/4, -x+1/4, y+1/2'
'-z+3/4, x, -y+3/4'
'y+1/2, z, x+1/2'
'-y+3/4, z, -x+3/4'
'y+1/2, -z+1/4, -x+3/4'
'-y+3/4, -z+1/4, x+1/2'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y+1/2, -z+1/4'
'x+1/2, -y+3/4, -z+1/4'
'z+1/2, x+1/2, y'
'z+1/2, -x+3/4, -y+1/4'
'-z+3/4, -x+3/4, y'
'-z+3/4, x+1/2, -y+1/4'
'y+1/2, z+1/2, x'
'-y+3/4, z+1/2, -x+1/4'
'y+1/2, -z+3/4, -x+1/4'
'-y+3/4, -z+3/4, x'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y, z-1/4'
'-x, y-1/4, z-1/4'
'-z, -x, -y'
'-z, x-1/4, y-1/4'
'z-1/4, x-1/4, -y'
'z-1/4, -x, y-1/4'
'-y, -z, -x'
'y-1/4, -z, x-1/4'
'-y, z-1/4, x-1/4'
'y-1/4, z-1/4, -x'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'x-1/4, -y+1/2, z+1/4'
'-x, y+1/4, z+1/4'
'-z, -x+1/2, -y+1/2'
'-z, x+1/4, y+1/4'
'z-1/4, x+1/4, -y+1/2'
'z-1/4, -x+1/2, y+1/4'
'-y, -z+1/2, -x+1/2'
'y-1/4, -z+1/2, x+1/4'
'-y, z+1/4, x+1/4'
'y-1/4, z+1/4, -x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'x+1/4, -y, z+1/4'
'-x+1/2, y-1/4, z+1/4'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x-1/4, y+1/4'
'z+1/4, x-1/4, -y+1/2'
'z+1/4, -x, y+1/4'
'-y+1/2, -z, -x+1/2'
'y+1/4, -z, x+1/4'
'-y+1/2, z-1/4, x+1/4'
'y+1/4, z-1/4, -x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'x+1/4, -y+1/2, z-1/4'
'-x+1/2, y+1/4, z-1/4'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/4, y-1/4'
'z+1/4, x+1/4, -y'
'z+1/4, -x+1/2, y-1/4'
'-y+1/2, -z+1/2, -x'
'y+1/4, -z+1/2, x-1/4'
'-y+1/2, z+1/4, x-1/4'
'y+1/4, z+1/4, -x'
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 -0.1250 0.3750 0.3750 0.0485(7) Uani 1 12 d S . .
Cl1 Cl 0.1250 0.1250 0.6250 0.061(3) Uani 1 12 d S . .
P1 P -0.05813(15) 0.30813(15) 0.44187(15) 0.0308(12) Uani 1 3 d S . .
N1 N -0.0475(5) 0.2100(6) 0.5397(6) 0.042(2) Uani 1 1 d . . .
C1 C -0.0961(6) 0.2480(7) 0.5001(8) 0.045(3) Uani 1 1 d . . .
H1A H -0.1251 0.2719 0.5305 0.054 Uiso 1 1 d R . .
H1B H -0.1232 0.2167 0.4750 0.054 Uiso 1 1 d R . .
C2 C -0.0045(8) 0.1693(6) 0.4960(7) 0.048(3) Uani 1 1 d . . .
H2A H 0.0225 0.1397 0.5230 0.057 Uiso 1 1 d R . .
H2B H -0.0327 0.1422 0.4676 0.057 Uiso 1 1 d R . .
O1 O -0.1263(6) 0.1250 0.6250 0.044(2) Uani 1 2 d S . .
H1O1 H -0.1137 0.1491 0.6539 0.16(10) Uiso 1 1 d R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Pt1 P1 109.5 27_455 38_455 ?
P1 Pt1 P1 109.5 27_455 . ?
P1 Pt1 P1 109.5 38_455 . ?
P1 Pt1 P1 109.5 27_455 16 ?
P1 Pt1 P1 109.471(1) 38_455 16 ?
P1 Pt1 P1 109.471(1) . 16 ?
C1 P1 C1 96.8(5) 24 . ?
C1 P1 C1 96.8(5) 24 30_455 ?
C1 P1 C1 96.8(5) . 30_455 ?
C1 P1 Pt1 120.3(4) 24 . ?
C1 P1 Pt1 120.3(4) . . ?
C1 P1 Pt1 120.3(4) 30_455 . ?
C2 N1 C1 110.7(12) . . ?
C2 N1 C2 108.5(13) . 30_455 ?
C1 N1 C2 112.1(10) . 30_455 ?
N1 C1 P1 114.0(8) . . ?
N1 C2 N1 113.0(10) . 24 ?
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 P1 2.299(5) 27_455 ?
Pt1 P1 2.299(5) 38_455 ?
Pt1 P1 2.299(5) . ?
Pt1 P1 2.299(5) 16 ?
P1 C1 1.825(12) 24 ?
P1 C1 1.825(12) . ?
P1 C1 1.825(12) 30_455 ?
N1 C2 1.460(18) . ?
N1 C1 1.455(14) . ?
N1 C2 1.478(18) 30_455 ?
C2 N1 1.478(18) 24 ?
