#------------------------------------------------------------------------------
#$Date: 2018-09-03 18:38:49 +0200 (lun 03 de sep de 2018) $
#$Revision: 210357 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/81/7118103.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_7118103
loop_
_publ_author_name
'Laura Ortega-Moreno'
'Riccardo Peloso'
'Celia Maya'
'Andres Suarez'
'Ernesto Carmona'
_publ_section_title
;
 Platinum(0) olefin complexes of a bulky terphenylphosphine ligand.
 Synthetic, structural and reactivity studies
;
_journal_name_full               Chem.Commun.
_journal_page_first              17008
_journal_paper_doi               10.1039/C5cc07308A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C99 H129 O3 P3 Pt3'
_chemical_formula_weight         2045.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-30 deposited with the CCDC.
2015-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   18.9177(4)
_cell_length_b                   18.9177(4)
_cell_length_c                   17.4660(4)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      22.20
_cell_measurement_theta_min      2.50
_cell_volume                     5413.3(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      95(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43366
_diffrn_reflns_theta_full        22.25
_diffrn_reflns_theta_max         22.25
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    2.150
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.6331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical
 X-ray Solutions, Madison, Wisconsin, USA. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.931
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.644
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         4797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.644
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+4.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0830
_reflns_number_gt                4083
_reflns_number_total             4797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc07308a2.cif
_cod_data_source_block           4
_cod_depositor_comments
;

2018-09-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         1022.60
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      P6(3)/m
_cod_original_formula_sum        'C49.50 H64.50 O1.50 P1.50 Pt1.50'
_cod_database_code               7118103
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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_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 0.575509(8) 0.270731(8) 0.7500 0.01334(7) Uani 1 2 d S . .
P1 P 0.44479(6) 0.16748(5) 0.7500 0.01372(18) Uani 1 2 d S . .
C21 C 0.6248(2) 0.1942(2) 0.7500 0.0163(7) Uani 1 2 d S . .
O2 O 0.60164(15) 0.12507(18) 0.7500 0.0181(5) Uani 1 2 d S . .
C4 C 0.3663(2) 0.1983(2) 0.7500 0.0137(6) Uani 1 2 d S . .
C9 C 0.28900(16) 0.10893(16) 0.57880(15) 0.0175(5) Uani 1 1 d . . .
C8 C 0.34827(16) 0.18810(16) 0.60258(15) 0.0166(5) Uani 1 1 d . . .
C10 C 0.29684(17) 0.08178(17) 0.50750(17) 0.0234(6) Uani 1 1 d . . .
H10 H 0.2576 0.0284 0.4912 0.028 Uiso 1 1 calc R . .
C5 C 0.33970(15) 0.21682(15) 0.68035(15) 0.0163(5) Uani 1 1 d . . .
C3 C 0.42544(16) 0.09649(16) 0.67152(16) 0.0214(5) Uani 1 1 d . . .
H3A H 0.4607 0.0726 0.6771 0.032 Uiso 1 1 calc R . .
H3B H 0.4371 0.1257 0.6227 0.032 Uiso 1 1 calc R . .
H3C H 0.3681 0.0530 0.6726 0.032 Uiso 1 1 calc R . .
C17 C 0.47164(16) 0.32858(16) 0.57271(16) 0.0212(5) Uani 1 1 d . . .
H17 H 0.4656 0.3363 0.6285 0.025 Uiso 1 1 calc R . .
C13 C 0.41145(16) 0.24040(16) 0.55231(15) 0.0190(5) Uani 1 1 d . . .
C18 C 0.55976(18) 0.35109(18) 0.55819(17) 0.0260(6) Uani 1 1 d . . .
H18A H 0.5723 0.3145 0.5874 0.039 Uiso 1 1 calc R . .
H18B H 0.5963 0.4076 0.5743 0.039 Uiso 1 1 calc R . .
H18C H 0.5675 0.3457 0.5035 0.039 Uiso 1 1 calc R . .
C14 C 0.21598(17) 0.05458(17) 0.62945(17) 0.0243(6) Uani 1 1 d . . .
H14 H 0.2314 0.0728 0.6837 0.029 Uiso 1 1 calc R . .
C6 C 0.29613(18) 0.25803(17) 0.68188(17) 0.0233(6) Uani 1 1 d . . .
H6 H 0.2805 0.2715 0.6348 0.028 Uiso 1 1 calc R . .
C11 C 0.36108(18) 0.13130(19) 0.45942(17) 0.0270(6) Uani 1 1 d . . .
H11 H 0.3668 0.1112 0.4114 0.032 Uiso 1 1 calc R . .
C12 C 0.41676(18) 0.21006(18) 0.48166(16) 0.0244(6) Uani 1 1 d . . .
H12 H 0.4597 0.2442 0.4477 0.029 Uiso 1 1 calc R . .
C15 C 0.19040(19) -0.03613(18) 0.6251(2) 0.0331(7) Uani 1 1 d . . .
H15A H 0.1679 -0.0574 0.5743 0.050 Uiso 1 1 calc R . .
H15B H 0.1489 -0.0665 0.6642 0.050 Uiso 1 1 calc R . .
H15C H 0.2381 -0.0424 0.6342 0.050 Uiso 1 1 calc R . .
C7 C 0.2747(3) 0.2802(3) 0.7500 0.0282(9) Uani 1 2 d S . .
H7 H 0.2462 0.3097 0.7500 0.034 Uiso 1 2 calc SR . .
C19 C 0.4516(2) 0.38547(19) 0.5277(2) 0.0365(8) Uani 1 1 d . . .
H19A H 0.4570 0.3787 0.4728 0.055 Uiso 1 1 calc R . .
H19B H 0.4894 0.4421 0.5425 0.055 Uiso 1 1 calc R . .
H19C H 0.3955 0.3721 0.5390 0.055 Uiso 1 1 calc R . .
C16 C 0.1428(2) 0.0650(2) 0.6084(2) 0.0397(8) Uani 1 1 d . . .
H16A H 0.1579 0.1224 0.6145 0.060 Uiso 1 1 calc R . .
H16B H 0.0968 0.0310 0.6421 0.060 Uiso 1 1 calc R . .
H16C H 0.1272 0.0484 0.5551 0.060 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 0.0015 0.0009 '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'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0667 0.0580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -0.6812 5.7081 '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
C21 Pt1 C21 159.91(14) 3_665 .
C21 Pt1 P1 105.72(10) 3_665 .
C21 Pt1 P1 94.37(11) . .
C21 Pt1 Pt1 50.62(10) 3_665 3_665
C21 Pt1 Pt1 109.29(10) . 3_665
P1 Pt1 Pt1 156.34(2) . 3_665
C21 Pt1 Pt1 110.62(10) 3_665 2_655
C21 Pt1 Pt1 49.29(10) . 2_655
P1 Pt1 Pt1 143.66(2) . 2_655
Pt1 Pt1 Pt1 60.0 3_665 2_655
C3 P1 C3 97.48(19) 10_557 .
C3 P1 C4 109.60(11) 10_557 .
C3 P1 C4 109.60(11) . .
C3 P1 Pt1 111.52(9) 10_557 .
C3 P1 Pt1 111.52(9) . .
C4 P1 Pt1 115.63(11) . .
O2 C21 Pt1 142.0(3) . 2_655
O2 C21 Pt1 137.9(3) . .
Pt1 C21 Pt1 80.09(14) 2_655 .
C5 C4 C5 117.1(3) . 10_557
C5 C4 P1 121.07(16) . .
C5 C4 P1 121.07(16) 10_557 .
C10 C9 C8 118.9(3) . .
C10 C9 C14 120.1(2) . .
C8 C9 C14 121.0(2) . .
C9 C8 C13 120.3(2) . .
C9 C8 C5 118.5(2) . .
C13 C8 C5 121.0(2) . .
C9 C10 C11 121.0(3) . .
C6 C5 C4 120.2(3) . .
C6 C5 C8 115.0(2) . .
C4 C5 C8 124.6(2) . .
C13 C17 C18 112.5(2) . .
C13 C17 C19 109.9(2) . .
C18 C17 C19 109.9(2) . .
C12 C13 C8 118.3(2) . .
C12 C13 C17 119.6(2) . .
C8 C13 C17 122.0(2) . .
C9 C14 C15 113.5(2) . .
C9 C14 C16 110.2(2) . .
C15 C14 C16 109.3(2) . .
C7 C6 C5 122.1(3) . .
C12 C11 C10 119.7(3) . .
C11 C12 C13 121.5(3) . .
C6 C7 C6 118.1(4) . 10_557
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 C21 2.036(4) 3_665
Pt1 C21 2.076(4) .
Pt1 P1 2.2584(9) .
Pt1 Pt1 2.6462(2) 3_665
Pt1 Pt1 2.6462(2) 2_655
P1 C3 1.823(3) 10_557
P1 C3 1.823(3) .
P1 C4 1.847(4) .
C21 O2 1.154(5) .
C21 Pt1 2.036(4) 2_655
C4 C5 1.426(3) .
C4 C5 1.426(3) 10_557
C9 C10 1.383(4) .
C9 C8 1.412(4) .
C9 C14 1.526(4) .
C8 C13 1.413(4) .
C8 C5 1.501(4) .
C10 C11 1.386(4) .
C5 C6 1.389(4) .
C17 C13 1.519(4) .
C17 C18 1.521(4) .
C17 C19 1.526(4) .
C13 C12 1.386(4) .
C14 C15 1.534(4) .
C14 C16 1.537(4) .
C6 C7 1.388(3) .
C11 C12 1.382(4) .
C7 C6 1.388(3) 10_557
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.667 0.333 0.250 630 179 ' '
2 0.000 0.000 0.250 44 7 ' '
3 0.333 0.667 0.750 630 180 ' '
4 0.000 0.000 0.750 44 7 ' '
