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#$Date: 2019-11-25 06:37:29 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240250 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/95/4129552.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_4129552
loop_
_publ_author_name
'Prack, Ernest'
'O'Keefe, Christopher A'
'Moore, Jeremy K.'
'Lai, Angel'
'Lough, Alan J.'
'Macdonald, Peter M.'
'Conradi, Mark S.'
'Schurko, Robert W.'
'Fekl, Ulrich'
_publ_section_title
;
 A Molecular Rotor Possessing an H-M-H "Spoke" on a P-M-P
 "Axle": A Platinum(II) trans-Dihydride Spins Rapidly Even at 75
 K.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13464
_journal_page_last               13467
_journal_paper_doi               10.1021/jacs.5b08213
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C24 H56 P2 Pt'
_chemical_formula_sum            'C24 H56 P2 Pt'
_chemical_formula_weight         601.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.717(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4834(12)
_cell_length_b                   13.6675(19)
_cell_length_c                   11.9574(16)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    147(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.27
_cell_volume                     1381.7(3)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      147(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX-DUO CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            69610
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.558
_diffrn_reflns_theta_min         2.267
_diffrn_source
'sealed tube with Bruker Triumph monochormator'
_exptl_absorpt_coefficient_mu    5.201
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       needle
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         3185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0136
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0059P)²+1.1770P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0278
_refine_ls_wR_factor_ref         0.0302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2658
_reflns_number_total             3185
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja5b08213_si_002.cif
_cod_data_source_block           d1389
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4129552
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.423
_shelx_estimated_absorpt_t_max   0.745
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pt1 Pt 0.5000 0.5000 0.5000 0.01640(3) Uani 1 2 d S . P
H1PT H 0.344(5) 0.517(3) 0.475(3) 0.110(14) Uiso 1 1 d . . .
P1 P 0.44519(5) 0.39230(3) 0.63697(4) 0.01632(9) Uani 1 1 d . . .
C1 C 0.5276(3) 0.26485(15) 0.61045(18) 0.0267(4) Uani 1 1 d . . .
C2 C 0.4233(3) 0.21540(18) 0.5155(2) 0.0434(6) Uani 1 1 d . . .
H2A H 0.4757 0.1560 0.4914 0.065 Uiso 1 1 calc R U .
H2B H 0.4068 0.2605 0.4519 0.065 Uiso 1 1 calc R U .
H2C H 0.3209 0.1982 0.5425 0.065 Uiso 1 1 calc R U .
C3 C 0.5411(3) 0.19587(16) 0.7121(2) 0.0393(6) Uani 1 1 d . . .
H3A H 0.5719 0.1305 0.6882 0.059 Uiso 1 1 calc R U .
H3B H 0.4388 0.1921 0.7444 0.059 Uiso 1 1 calc R U .
H3C H 0.6213 0.2209 0.7685 0.059 Uiso 1 1 calc R U .
C4 C 0.6916(3) 0.2735(2) 0.5655(2) 0.0419(6) Uani 1 1 d . . .
H4A H 0.7312 0.2081 0.5492 0.063 Uiso 1 1 calc R U .
H4B H 0.7648 0.3053 0.6220 0.063 Uiso 1 1 calc R U .
H4C H 0.6836 0.3127 0.4966 0.063 Uiso 1 1 calc R U .
C5 C 0.5402(2) 0.43716(15) 0.77811(17) 0.0250(4) Uani 1 1 d . . .
C6 C 0.4807(3) 0.38965(18) 0.88311(17) 0.0350(5) Uani 1 1 d . . .
H6A H 0.5449 0.4125 0.9499 0.052 Uiso 1 1 calc R U .
H6B H 0.4892 0.3183 0.8775 0.052 Uiso 1 1 calc R U .
H6C H 0.3699 0.4078 0.8890 0.052 Uiso 1 1 calc R U .
C7 C 0.5176(3) 0.54867(18) 0.7859(2) 0.0465(7) Uani 1 1 d . . .
H7A H 0.5785 0.5735 0.8532 0.070 Uiso 1 1 calc R U .
H7B H 0.4053 0.5634 0.7904 0.070 Uiso 1 1 calc R U .
H7C H 0.5548 0.5800 0.7192 0.070 Uiso 1 1 calc R U .
C8 C 0.7197(3) 0.42166(19) 0.78158(19) 0.0368(5) Uani 1 1 d . . .
H8A H 0.7710 0.4543 0.8478 0.055 Uiso 1 1 calc R U .
H8B H 0.7595 0.4493 0.7137 0.055 Uiso 1 1 calc R U .
H8C H 0.7431 0.3515 0.7854 0.055 Uiso 1 1 calc R U .
C9 C 0.2229(2) 0.38047(16) 0.64859(18) 0.0264(4) Uani 1 1 d . . .
C10 C 0.1716(3) 0.29411(19) 0.7201(2) 0.0420(6) Uani 1 1 d . . .
H10A H 0.0574 0.2977 0.7269 0.063 Uiso 1 1 calc R U .
H10B H 0.2278 0.2974 0.7950 0.063 Uiso 1 1 calc R U .
H10C H 0.1970 0.2323 0.6841 0.063 Uiso 1 1 calc R U .
C11 C 0.1618(3) 0.47550(17) 0.6976(2) 0.0390(6) Uani 1 1 d . . .
H11A H 0.0459 0.4755 0.6901 0.059 Uiso 1 1 calc R U .
H11B H 0.2011 0.5315 0.6569 0.059 Uiso 1 1 calc R U .
H11C H 0.1995 0.4802 0.7771 0.059 Uiso 1 1 calc R U .
C12 C 0.1368(3) 0.3712(2) 0.5307(2) 0.0454(6) Uani 1 1 d . . .
H12A H 0.0224 0.3764 0.5360 0.068 Uiso 1 1 calc R U .
H12B H 0.1613 0.3076 0.4985 0.068 Uiso 1 1 calc R U .
H12C H 0.1717 0.4236 0.4826 0.068 Uiso 1 1 calc R U .
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'
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
P1 Pt1 P1 179.999(16) 3_666
P1 Pt1 H1PT 89.0(16) 3_666
P1 Pt1 H1PT 91.0(16) .
C9 P1 C5 108.09(9) .
C9 P1 C1 108.15(9) .
C5 P1 C1 107.77(9) .
C9 P1 Pt1 111.61(7) .
C5 P1 Pt1 109.36(7) .
C1 P1 Pt1 111.72(7) .
C3 C1 C4 108.26(19) .
C3 C1 C2 108.42(19) .
C4 C1 C2 104.95(19) .
C3 C1 P1 115.63(15) .
C4 C1 P1 109.96(15) .
C2 C1 P1 109.07(15) .
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 .
C1 C3 H3A 109.5 .
C1 C3 H3B 109.5 .
H3A C3 H3B 109.5 .
C1 C3 H3C 109.5 .
H3A C3 H3C 109.5 .
H3B C3 H3C 109.5 .
C1 C4 H4A 109.5 .
C1 C4 H4B 109.5 .
H4A C4 H4B 109.5 .
C1 C4 H4C 109.5 .
H4A C4 H4C 109.5 .
H4B C4 H4C 109.5 .
C8 C5 C6 108.17(18) .
C8 C5 C7 105.25(19) .
C6 C5 C7 108.54(19) .
C8 C5 P1 108.98(15) .
C6 C5 P1 116.32(15) .
C7 C5 P1 109.00(15) .
C5 C6 H6A 109.5 .
C5 C6 H6B 109.5 .
H6A C6 H6B 109.5 .
C5 C6 H6C 109.5 .
H6A C6 H6C 109.5 .
H6B C6 H6C 109.5 .
C5 C7 H7A 109.5 .
C5 C7 H7B 109.5 .
H7A C7 H7B 109.5 .
C5 C7 H7C 109.5 .
H7A C7 H7C 109.5 .
H7B C7 H7C 109.5 .
C5 C8 H8A 109.5 .
C5 C8 H8B 109.5 .
H8A C8 H8B 109.5 .
C5 C8 H8C 109.5 .
H8A C8 H8C 109.5 .
H8B C8 H8C 109.5 .
C11 C9 C12 105.68(19) .
C11 C9 C10 108.49(18) .
C12 C9 C10 108.11(19) .
C11 C9 P1 108.84(15) .
C12 C9 P1 109.74(15) .
C10 C9 P1 115.52(15) .
C9 C10 H10A 109.5 .
C9 C10 H10B 109.5 .
H10A C10 H10B 109.5 .
C9 C10 H10C 109.5 .
H10A C10 H10C 109.5 .
H10B C10 H10C 109.5 .
C9 C11 H11A 109.5 .
C9 C11 H11B 109.5 .
H11A C11 H11B 109.5 .
C9 C11 H11C 109.5 .
H11A C11 H11C 109.5 .
H11B C11 H11C 109.5 .
C9 C12 H12A 109.5 .
C9 C12 H12B 109.5 .
H12A C12 H12B 109.5 .
C9 C12 H12C 109.5 .
H12A C12 H12C 109.5 .
H12B C12 H12C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 P1 2.2782(5) 3_666
Pt1 P1 2.2783(5) .
Pt1 H1PT 1.35(4) .
P1 C9 1.909(2) .
P1 C5 1.911(2) .
P1 C1 1.913(2) .
C1 C3 1.535(3) .
C1 C4 1.537(3) .
C1 C2 1.538(3) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 C8 1.534(3) .
C5 C6 1.535(3) .
C5 C7 1.540(3) .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C11 1.532(3) .
C9 C12 1.539(3) .
C9 C10 1.541(3) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
