#------------------------------------------------------------------------------
#$Date: 2016-03-21 11:09:19 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178682 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/93/4079383.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_4079383
loop_
_publ_author_name
'Guino-o, Marites A.'
'Zureick, Andrew H.'
'Blank, Natalia F.'
'Anderson, Brian J.'
'Chapp, Timothy W.'
'Kim, Youngmin'
'Glueck, David S.'
'Rheingold, Arnold L.'
_publ_section_title
;
 Synthesis and Structure of Platinum Bis(phospholane) Complexes
 Pt(diphos*)(R)(X), Catalyst Precursors for Asymmetric Phosphine
 Alkylation
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              6900
_journal_paper_doi               10.1021/om300704e
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C14 H28 I2 P2 Pt'
_chemical_formula_weight         707.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           80
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4bw'
_symmetry_space_group_name_H-M   'I 41'
_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                   19.7843(10)
_cell_length_b                   19.7843(10)
_cell_length_c                   10.6175(10)
_cell_measurement_reflns_used    7186
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.91
_cell_volume                     4155.9(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11577
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    9.867
_exptl_absorpt_correction_T_max  0.2961
_exptl_absorpt_correction_T_min  0.1412
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.009(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3774
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0269
_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)+(0.0010P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0597
_reflns_number_gt                3613
_reflns_number_total             3774
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300704e_si_002.cif
_cod_data_source_block           glu352
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      I4(1)
_cod_database_code               4079383
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
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
Pt1 Pt 0.768422(14) 0.498098(14) 0.03001(3) 0.02168(8) Uani 1 1 d .
I1 I 0.88407(2) 0.51043(3) 0.15894(5) 0.02637(12) Uani 1 1 d .
I2 I 0.82948(3) 0.51220(3) -0.19052(5) 0.03352(14) Uani 1 1 d .
P1 P 0.67061(10) 0.47734(11) -0.06838(19) 0.0252(5) Uani 1 1 d .
P2 P 0.70817(11) 0.49573(11) 0.20824(19) 0.0250(4) Uani 1 1 d .
C1 C 0.6028(4) 0.4958(4) 0.0433(8) 0.0281(18) Uani 1 1 d .
H1A H 0.5958 0.5453 0.0495 0.034 Uiso 1 1 calc R
H1B H 0.5601 0.4748 0.0147 0.034 Uiso 1 1 calc R
C2 C 0.6230(4) 0.4676(4) 0.1697(8) 0.0301(19) Uani 1 1 d .
H2A H 0.6215 0.4176 0.1673 0.036 Uiso 1 1 calc R
H2B H 0.5909 0.4833 0.2351 0.036 Uiso 1 1 calc R
C3 C 0.6204(5) 0.5860(4) -0.2156(9) 0.047(2) Uani 1 1 d .
H3A H 0.6093 0.6015 -0.3008 0.071 Uiso 1 1 calc R
H3B H 0.6563 0.6145 -0.1805 0.071 Uiso 1 1 calc R
H3C H 0.5801 0.5890 -0.1622 0.071 Uiso 1 1 calc R
C4 C 0.6440(4) 0.5143(4) -0.2209(8) 0.0341(19) Uani 1 1 d .
H4A H 0.6840 0.5128 -0.2784 0.041 Uiso 1 1 calc R
C5 C 0.5937(4) 0.4628(5) -0.2683(8) 0.041(2) Uani 1 1 d .
H5A H 0.5839 0.4707 -0.3586 0.049 Uiso 1 1 calc R
H5B H 0.5509 0.4663 -0.2205 0.049 Uiso 1 1 calc R
C6 C 0.6254(5) 0.3919(5) -0.2499(9) 0.053(3) Uani 1 1 d .
H6A H 0.6603 0.3838 -0.3149 0.064 Uiso 1 1 calc R
H6B H 0.5902 0.3567 -0.2582 0.064 Uiso 1 1 calc R
C7 C 0.6579(4) 0.3886(4) -0.1158(8) 0.034(2) Uani 1 1 d .
H7A H 0.6230 0.3693 -0.0581 0.041 Uiso 1 1 calc R
C8 C 0.7183(5) 0.3435(4) -0.1077(9) 0.041(2) Uani 1 1 d .
H8A H 0.7056 0.2975 -0.1327 0.061 Uiso 1 1 calc R
H8B H 0.7352 0.3430 -0.0209 0.061 Uiso 1 1 calc R
H8C H 0.7537 0.3604 -0.1641 0.061 Uiso 1 1 calc R
C9 C 0.7282(6) 0.6383(5) 0.2293(11) 0.060(3) Uani 1 1 d .
H9A H 0.7200 0.6783 0.2815 0.090 Uiso 1 1 calc R
H9B H 0.7071 0.6446 0.1466 0.090 Uiso 1 1 calc R
H9C H 0.7770 0.6318 0.2187 0.090 Uiso 1 1 calc R
C10 C 0.6984(4) 0.5773(4) 0.2918(8) 0.038(2) Uani 1 1 d .
H10A H 0.6488 0.5858 0.3006 0.045 Uiso 1 1 calc R
C11 C 0.7259(5) 0.5626(6) 0.4250(10) 0.061(3) Uani 1 1 d .
H11A H 0.7031 0.5918 0.4876 0.073 Uiso 1 1 calc R
H11B H 0.7751 0.5718 0.4283 0.073 Uiso 1 1 calc R
C12 C 0.7122(5) 0.4874(6) 0.4553(9) 0.059(3) Uani 1 1 d .
H12A H 0.7368 0.4739 0.5325 0.070 Uiso 1 1 calc R
H12B H 0.6633 0.4799 0.4691 0.070 Uiso 1 1 calc R
C13 C 0.7364(4) 0.4464(5) 0.3444(7) 0.035(2) Uani 1 1 d .
H13A H 0.7870 0.4470 0.3452 0.042 Uiso 1 1 calc R
C14 C 0.7138(5) 0.3729(5) 0.3479(9) 0.050(3) Uani 1 1 d .
H14A H 0.7312 0.3513 0.4245 0.075 Uiso 1 1 calc R
H14B H 0.7315 0.3492 0.2738 0.075 Uiso 1 1 calc R
H14C H 0.6644 0.3708 0.3477 0.075 Uiso 1 1 calc 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
P1 Pt1 P2 86.00(8)
P1 Pt1 I2 90.06(5)
P2 Pt1 I2 173.10(6)
P1 Pt1 I1 174.09(6)
P2 Pt1 I1 91.42(6)
I2 Pt1 I1 93.016(19)
C1 P1 C7 105.5(4)
C1 P1 C4 106.2(4)
C7 P1 C4 95.7(4)
C1 P1 Pt1 107.2(3)
C7 P1 Pt1 114.8(3)
C4 P1 Pt1 125.5(3)
C2 P2 C13 107.3(4)
C2 P2 C10 106.1(4)
C13 P2 C10 96.8(4)
C2 P2 Pt1 108.0(3)
C13 P2 Pt1 121.1(3)
C10 P2 Pt1 116.3(3)
C2 C1 P1 108.0(5)
C1 C2 P2 109.4(6)
C3 C4 C5 116.5(7)
C3 C4 P1 115.5(6)
C5 C4 P1 102.3(6)
C4 C5 C6 107.5(7)
C5 C6 C7 108.7(7)
C8 C7 C6 114.0(7)
C8 C7 P1 116.3(6)
C6 C7 P1 105.3(6)
C9 C10 C11 114.9(8)
C9 C10 P2 116.6(6)
C11 C10 P2 103.7(6)
C10 C11 C12 108.1(8)
C13 C12 C11 107.4(8)
C12 C13 C14 113.7(8)
C12 C13 P2 103.5(7)
C14 C13 P2 116.0(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pt1 P1 2.237(2)
Pt1 P2 2.237(2)
Pt1 I2 2.6494(6)
Pt1 I1 2.6775(6)
P1 C1 1.827(8)
P1 C7 1.845(8)
P1 C4 1.853(8)
P2 C2 1.822(8)
P2 C13 1.832(8)
P2 C10 1.852(8)
C1 C2 1.508(11)
C3 C4 1.494(11)
C4 C5 1.512(12)
C5 C6 1.549(14)
C6 C7 1.563(12)
C7 C8 1.493(12)
C9 C10 1.497(13)
C10 C11 1.543(14)
C11 C12 1.546(15)
C12 C13 1.508(13)
C13 C14 1.522(13)
