#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:08:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179314 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/11/4321164.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_4321164
loop_
_publ_author_name
'Kent D. Redwine'
'William L. Wilson'
'Donald G. Moses'
'Vincent J. Catalano'
'John H. Nelson'
_publ_section_title
;
 Cooperative Diastereoselectivity of Palladium- and Platinum-Promoted
 Intramolecular [4+2] Diels-Alder Cycloaddition Reactions of
 3,4-Dimethyl-1-phenylphosphole
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3392
_journal_page_last               3402
_journal_paper_doi               10.1021/ic990885j
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C34 H44 B2 F8 N2 O2 P2 Pt'
_chemical_formula_weight         943.36
_chemical_name_common            2b
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.70(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.961(7)
_cell_length_b                   10.583(3)
_cell_length_c                   19.869(4)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      16.55
_cell_measurement_theta_min      4.55
_cell_volume                     3733(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω 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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3090
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        2.97
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.918
_exptl_absorpt_correction_T_max  0.9907
_exptl_absorpt_correction_T_min  0.3743
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       lozenge
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          .22
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .51
_refine_diff_density_max         1.055
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00229(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.070
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         2445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_obs          0.0339
_refine_ls_shift/esd_max         0.012
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0513P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0796
_refine_ls_wR_factor_obs         0.0762
_reflns_number_observed          2166
_reflns_number_total             2445
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990885j_4.cif
_cod_data_source_block           122
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3733.2(19)
_cod_database_code               4321164
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'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pt1 Pt 0.0000 0.09159(3) 0.7500 0.0285(2) Uani 1 d S .
P1 P -0.01686(9) 0.2300(2) 0.66734(8) 0.0297(4) Uani 1 d . .
O1 O -0.0330(3) -0.0570(4) 0.6828(2) 0.0393(11) Uani 1 d . .
N1 N -0.1326(3) -0.1445(6) 0.6216(3) 0.0407(14) Uani 1 d . .
C1 C -0.0236(4) 0.1439(6) 0.5868(3) 0.034(2) Uani 1 d . .
H1A H 0.0207(4) 0.0938(6) 0.5802(3) 0.041 Uiso 1 calc R .
C2 C -0.0433(4) 0.2515(7) 0.5375(3) 0.041(2) Uani 1 d . .
C3 C -0.0912(4) 0.3317(7) 0.5604(3) 0.040(2) Uani 1 d . .
C4 C -0.1095(3) 0.2895(7) 0.6287(3) 0.037(2) Uani 1 d . .
H4A H -0.1317(3) 0.3540(7) 0.6550(3) 0.045 Uiso 1 calc R .
C5 C -0.1529(4) 0.1618(7) 0.6189(3) 0.040(2) Uani 1 d . .
H5A H -0.1991(4) 0.1714(7) 0.5871(3) 0.048 Uiso 1 calc R .
H5B H -0.1653(4) 0.1315(7) 0.6620(3) 0.048 Uiso 1 calc R .
C6 C -0.0975(4) 0.0678(6) 0.5901(3) 0.035(2) Uani 1 d . .
H6A H -0.1195(4) 0.0432(6) 0.5438(3) 0.042 Uiso 1 calc R .
C7 C -0.0860(4) -0.0484(6) 0.6333(3) 0.034(2) Uani 1 d . .
C8 C -0.0128(5) 0.2540(8) 0.4717(4) 0.068(2) Uani 1 d . .
H8A H 0.0408(7) 0.2421(57) 0.4803(5) 0.102 Uiso 1 calc R .
H8B H -0.0241(30) 0.3340(24) 0.4497(15) 0.102 Uiso 1 calc R .
H8C H -0.0355(26) 0.1875(38) 0.4427(13) 0.102 Uiso 1 calc R .
C9 C -0.1298(5) 0.4441(7) 0.5242(4) 0.062(2) Uani 1 d . .
H9A H -0.1213(27) 0.5172(13) 0.5529(12) 0.093 Uiso 1 calc R .
H9B H -0.1829(7) 0.4280(22) 0.5138(26) 0.093 Uiso 1 calc R .
H9C H -0.1097(23) 0.4588(34) 0.4828(15) 0.093 Uiso 1 calc R .
C10 C -0.1949(4) -0.1529(8) 0.5647(4) 0.061(2) Uani 1 d . .
H10A H -0.2313(15) -0.2133(36) 0.5754(12) 0.092 Uiso 1 calc R .
H10B H -0.1758(6) -0.1793(47) 0.5243(7) 0.092 Uiso 1 calc R .
H10C H -0.2185(19) -0.0717(14) 0.5570(17) 0.092 Uiso 1 calc R .
C11 C -0.1233(4) -0.2507(7) 0.6683(4) 0.057(2) Uani 1 d . .
H11A H -0.1667(14) -0.3046(26) 0.6596(18) 0.086 Uiso 1 calc R .
H11B H -0.1179(29) -0.2201(7) 0.7143(4) 0.086 Uiso 1 calc R .
H11C H -0.0791(17) -0.2975(29) 0.6619(19) 0.086 Uiso 1 calc R .
C12 C 0.0529(4) 0.3535(7) 0.6748(3) 0.036(2) Uani 1 d . .
C13 C 0.1280(4) 0.3207(8) 0.6888(4) 0.053(2) Uani 1 d . .
H13A H 0.1424(4) 0.2362(8) 0.6915(4) 0.064 Uiso 1 calc R .
C14 C 0.1826(5) 0.4173(9) 0.6990(5) 0.068(3) Uani 1 d . .
H14A H 0.2334(5) 0.3964(9) 0.7084(5) 0.081 Uiso 1 calc R .
C15 C 0.1613(6) 0.5417(9) 0.6951(4) 0.065(2) Uani 1 d . .
H15A H 0.1977(6) 0.6048(9) 0.7021(4) 0.077 Uiso 1 calc R .
C16 C 0.0870(6) 0.5734(7) 0.6810(4) 0.060(2) Uani 1 d . .
H16A H 0.0728(6) 0.6580(7) 0.6780(4) 0.072 Uiso 1 calc R .
C17 C 0.0325(4) 0.4790(7) 0.6712(3) 0.046(2) Uani 1 d . .
H17A H -0.0182(4) 0.5009(7) 0.6621(3) 0.055 Uiso 1 calc R .
B1 B 0.8139(6) 0.0332(13) 0.3701(8) 0.073(3) Uani 1 d . .
F1 F 0.8506(20) 0.0599(39) 0.3259(16) 0.220(20) Uani 0.50 d P 1
F2 F 0.8581(22) -0.0246(48) 0.4123(19) 0.208(21) Uani 0.50 d P 1
F3 F 0.7947(16) 0.1321(25) 0.4099(18) 0.203(13) Uani 0.50 d P 1
F4 F 0.7491(4) -0.0287(8) 0.3633(4) 0.148(3) Uani 1 d . 1
F1A F 0.8407(12) -0.0073(19) 0.3087(12) 0.097(7) Uani 0.50 d P 2
F2A F 0.8649(16) -0.0008(31) 0.4276(14) 0.093(6) Uani 0.50 d P 2
F3A F 0.7978(13) 0.1575(15) 0.3583(11) 0.110(6) Uani 0.50 d P 2
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pt1 O1 82.4(2) 2_556 . ?
O1 Pt1 P1 91.74(13) 2_556 2_556 ?
O1 Pt1 P1 167.79(13) . 2_556 ?
O1 Pt1 P1 167.79(13) 2_556 . ?
O1 Pt1 P1 91.74(13) . . ?
P1 Pt1 P1 95.91(9) 2_556 . ?
C12 P1 C1 112.7(3) . . ?
C12 P1 C4 111.2(3) . . ?
C1 P1 C4 82.5(3) . . ?
C12 P1 Pt1 114.1(2) . . ?
C1 P1 Pt1 107.9(2) . . ?
C4 P1 Pt1 123.9(2) . . ?
C7 O1 Pt1 123.3(4) . . ?
C7 N1 C11 118.5(5) . . ?
C7 N1 C10 125.0(6) . . ?
C11 N1 C10 116.5(6) . . ?
C2 C1 C6 107.4(5) . . ?
C2 C1 P1 99.8(4) . . ?
C6 C1 P1 99.4(4) . . ?
C3 C2 C8 128.9(7) . . ?
C3 C2 C1 111.0(6) . . ?
C8 C2 C1 120.0(6) . . ?
C2 C3 C9 127.9(6) . . ?
C2 C3 C4 110.9(6) . . ?
C9 C3 C4 121.1(6) . . ?
C3 C4 C5 108.5(5) . . ?
C3 C4 P1 99.8(4) . . ?
C5 C4 P1 99.2(4) . . ?
C4 C5 C6 105.2(5) . . ?
C7 C6 C1 113.8(5) . . ?
C7 C6 C5 110.5(5) . . ?
C1 C6 C5 106.1(5) . . ?
O1 C7 N1 117.7(6) . . ?
O1 C7 C6 121.9(6) . . ?
N1 C7 C6 120.4(6) . . ?
C17 C12 C13 119.8(7) . . ?
C17 C12 P1 121.3(5) . . ?
C13 C12 P1 118.8(6) . . ?
C12 C13 C14 119.0(8) . . ?
C15 C14 C13 120.4(8) . . ?
C16 C15 C14 120.3(8) . . ?
C15 C16 C17 119.8(8) . . ?
C12 C17 C16 120.6(8) . . ?
F1 B1 F2 104.3(30) . . ?
F1 B1 F4 127.5(21) . . ?
F2 B1 F4 106.9(27) . . ?
F1 B1 F3 116.6(24) . . ?
F2 B1 F3 100.3(25) . . ?
F4 B1 F3 98.1(15) . . ?
F3A B1 F2A 119.1(19) . . ?
F3A B1 F1A 103.3(18) . . ?
F2A B1 F1A 110.7(17) . . ?
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 O1 2.090(4) 2_556 ?
Pt1 O1 2.091(4) . ?
Pt1 P1 2.187(2) 2_556 ?
Pt1 P1 2.187(2) . ?
P1 C12 1.801(7) . ?
P1 C1 1.830(6) . ?
P1 C4 1.835(6) . ?
O1 C7 1.265(8) . ?
N1 C7 1.316(9) . ?
N1 C11 1.450(9) . ?
N1 C10 1.469(9) . ?
C1 C2 1.509(9) . ?
C1 C6 1.563(9) . ?
C2 C3 1.336(9) . ?
C2 C8 1.493(9) . ?
C3 C9 1.504(10) . ?
C3 C4 1.512(9) . ?
C4 C5 1.558(9) . ?
C5 C6 1.575(9) . ?
C6 C7 1.495(9) . ?
C12 C17 1.378(10) . ?
C12 C13 1.380(10) . ?
C13 C14 1.410(11) . ?
C14 C15 1.370(11) . ?
C15 C16 1.364(13) . ?
C16 C17 1.391(10) . ?
B1 F1 1.21(3) . ?
B1 F2 1.23(4) . ?
B1 F4 1.325(13) . ?
B1 F3A 1.36(2) . ?
B1 F3 1.39(3) . ?
B1 F2A 1.40(3) . ?
B1 F1A 1.44(3) . ?
