#------------------------------------------------------------------------------
#$Date: 2019-11-24 05:42:04 +0200 (Sun, 24 Nov 2019) $
#$Revision: 236851 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/75/4087562.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_4087562
loop_
_publ_author_name
'Wickramasinghe, Lasantha A.'
'Sharp, Paul R.'
_publ_section_title
;
 Hydroxyl Radical Control through Hydrogen Bonding: Photolysis of
 Platinum(IV)hydroxido Complexes with Intramolecular H-Bonding
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3451
_journal_paper_doi               10.1021/acs.organomet.5b00292
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C20 H34 F3 N P2 Pt'
_chemical_formula_weight         602.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.853(4)
_cell_length_b                   13.165(4)
_cell_length_c                   14.310(4)
_cell_measurement_reflns_used    8841
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.21
_cell_volume                     2421.4(13)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_structure_refinement  'SHELXL-2015 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13930
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.662
_diffrn_reflns_theta_min         2.214
_exptl_absorpt_coefficient_mu    5.955
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 1185 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2926
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0153
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0133P)²+0.3996P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0356
_refine_ls_wR_factor_ref         0.0366
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                2615
_reflns_number_total             2926
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om5b00292_si_002.cif
_cod_data_source_block           Z:\X-Ray\Lasantha\PtL2RCN\work\PtCNcyc
_cod_original_cell_volume        2421.3(12)
_cod_database_code               4087562
_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   0.318
_shelx_estimated_absorpt_t_max   0.716
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, 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'
'-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_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 1.0000 0.62486(2) 0.25306(3) 0.01359(6) Uani 1 2 d S T P
P1 P 0.82218(8) 0.62460(7) 0.2598(2) 0.0166(3) Uani 1 1 d . . .
F1 F 1.0834(3) 1.0456(3) -0.0360(4) 0.0816(16) Uani 1 1 d . . .
N1 N 1.0000 0.4243(6) 0.3746(5) 0.0474(19) Uani 1 2 d S T P
C1 C 1.0000 0.7455(4) 0.1626(4) 0.0146(11) Uani 1 2 d S T P
F2 F 1.0000 0.9585(4) -0.1294(4) 0.0632(15) Uani 1 2 d S T P
C2 C 1.0000 0.8482(4) 0.1909(5) 0.0185(12) Uani 1 2 d S T P
H2 H 1.0000 0.8644 0.2556 0.022 Uiso 1 2 calc R U P
C3 C 1.0000 0.9261(5) 0.1249(5) 0.0206(14) Uani 1 2 d S T P
H3 H 1.0000 0.9948 0.1453 0.025 Uiso 1 2 calc R U P
C4 C 1.0000 0.9047(5) 0.0291(5) 0.0247(15) Uani 1 2 d S T P
C5 C 1.0000 0.8054(5) 0.0003(4) 0.0206(13) Uani 1 2 d S T P
H5 H 1.0000 0.7897 -0.0645 0.025 Uiso 1 2 calc R U P
C6 C 1.0000 0.7275(4) 0.0660(4) 0.0168(12) Uani 1 2 d S T P
H6 H 1.0000 0.6592 0.0446 0.020 Uiso 1 2 calc R U P
C7 C 1.0000 0.9919(6) -0.0381(6) 0.0371(19) Uani 1 2 d S T P
C8 C 0.7556(3) 0.7243(3) 0.1966(4) 0.0229(10) Uani 1 1 d . . .
H8A H 0.7820 0.7904 0.2194 0.028 Uiso 1 1 calc R U .
H8B H 0.7748 0.7187 0.1298 0.028 Uiso 1 1 calc R U .
C9 C 0.6372(4) 0.7256(4) 0.2034(4) 0.0345(12) Uani 1 1 d . . .
H9A H 0.6093 0.6612 0.1800 0.052 Uiso 1 1 calc R U .
H9B H 0.6098 0.7818 0.1658 0.052 Uiso 1 1 calc R U .
H9C H 0.6165 0.7348 0.2688 0.052 Uiso 1 1 calc R U .
C10 C 0.7772(4) 0.6360(3) 0.3807(4) 0.0284(11) Uani 1 1 d . . .
H10A H 0.7003 0.6322 0.3819 0.034 Uiso 1 1 calc R U .
H10B H 0.8046 0.5783 0.4176 0.034 Uiso 1 1 calc R U .
C11 C 0.8120(5) 0.7352(4) 0.4254(4) 0.0436(15) Uani 1 1 d . . .
H11A H 0.8880 0.7407 0.4217 0.065 Uiso 1 1 calc R U .
H11B H 0.7904 0.7364 0.4911 0.065 Uiso 1 1 calc R U .
H11C H 0.7802 0.7925 0.3923 0.065 Uiso 1 1 calc R U .
C12 C 0.7654(4) 0.5056(3) 0.2188(3) 0.0226(10) Uani 1 1 d . . .
H12A H 0.7947 0.4485 0.2554 0.027 Uiso 1 1 calc R U .
H12B H 0.6893 0.5070 0.2296 0.027 Uiso 1 1 calc R U .
C13 C 0.7867(4) 0.4877(4) 0.1145(3) 0.0311(11) Uani 1 1 d . . .
H13A H 0.7577 0.5440 0.0781 0.047 Uiso 1 1 calc R U .
H13B H 0.7540 0.4239 0.0949 0.047 Uiso 1 1 calc R U .
H13C H 0.8619 0.4838 0.1040 0.047 Uiso 1 1 calc R U .
C1N C 1.0000 0.4974(5) 0.3350(5) 0.0257(14) Uani 1 2 d S T P
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'
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
C1N Pt1 C1 175.8(3) . .
C1N Pt1 P1 88.54(5) . .
C1 Pt1 P1 91.60(5) . .
C1N Pt1 P1 88.54(5) . 3_755
C1 Pt1 P1 91.60(5) . 3_755
P1 Pt1 P1 175.13(16) . 3_755
C8 P1 C12 105.8(3) . .
C8 P1 C10 105.3(2) . .
C12 P1 C10 104.3(2) . .
C8 P1 Pt1 116.77(16) . .
C12 P1 Pt1 112.78(16) . .
C10 P1 Pt1 110.9(2) . .
C6 C1 C2 116.4(5) . .
C6 C1 Pt1 119.4(4) . .
C2 C1 Pt1 124.2(4) . .
C3 C2 C1 120.7(6) . .
C3 C2 H2 119.6 . .
C1 C2 H2 119.6 . .
C2 C3 C4 121.0(6) . .
C2 C3 H3 119.5 . .
C4 C3 H3 119.5 . .
C5 C4 C3 119.1(6) . .
C5 C4 C7 122.6(7) . .
C3 C4 C7 118.3(6) . .
C4 C5 C6 120.0(6) . .
C4 C5 H5 120.0 . .
C6 C5 H5 120.0 . .
C5 C6 C1 122.8(6) . .
C5 C6 H6 118.6 . .
C1 C6 H6 118.6 . .
F1 C7 F1 113.2(7) . 3_755
F1 C7 F2 101.4(5) . .
F1 C7 F2 101.4(5) 3_755 .
F1 C7 C4 114.0(4) . .
F1 C7 C4 114.0(4) 3_755 .
F2 C7 C4 111.3(7) . .
C9 C8 P1 116.7(3) . .
C9 C8 H8A 108.1 . .
P1 C8 H8A 108.1 . .
C9 C8 H8B 108.1 . .
P1 C8 H8B 108.1 . .
H8A C8 H8B 107.3 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C11 C10 P1 112.0(3) . .
C11 C10 H10A 109.2 . .
P1 C10 H10A 109.2 . .
C11 C10 H10B 109.2 . .
P1 C10 H10B 109.2 . .
H10A C10 H10B 107.9 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C13 C12 P1 111.9(3) . .
C13 C12 H12A 109.2 . .
P1 C12 H12A 109.2 . .
C13 C12 H12B 109.2 . .
P1 C12 H12B 109.2 . .
H12A C12 H12B 107.9 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
N1 C1N Pt1 175.6(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 C1N 2.047(7) .
Pt1 C1 2.049(6) .
Pt1 P1 2.2876(12) .
Pt1 P1 2.2876(12) 3_755
P1 C8 1.809(5) .
P1 C12 1.825(4) .
P1 C10 1.829(6) .
F1 C7 1.285(5) .
N1 C1N 1.117(9) .
C1 C6 1.402(8) .
C1 C2 1.411(8) .
F2 C7 1.379(10) .
C2 C3 1.394(9) .
C2 H2 0.9500 .
C3 C4 1.400(10) .
C3 H3 0.9500 .
C4 C5 1.372(9) .
C4 C7 1.497(9) .
C5 C6 1.392(8) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 F1 1.285(5) 3_755
C8 C9 1.524(6) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 C11 1.523(6) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 C13 1.536(6) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
