#------------------------------------------------------------------------------
#$Date: 2020-10-14 03:59:47 +0300 (Wed, 14 Oct 2020) $
#$Revision: 258351 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/93/1559346.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_1559346
loop_
_publ_author_name
'Poveda, Dionisio'
'Vivancos, Angela'
'Bautista, Delia'
'González-Herrero, Pablo'
_publ_section_title
;
 Visible light driven generation and alkyne insertion reactions of stable
 bis-cyclometalated Pt(IV) hydrides
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC04879H
_journal_year                    2020
_chemical_formula_sum            'C27 H27 Cl N2 O Pt'
_chemical_formula_weight         626.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2020-07-24 deposited with the CCDC.	2020-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.696(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4349(7)
_cell_length_b                   10.9885(6)
_cell_length_c                   16.2400(8)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      2.28
_cell_volume                     2363.3(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc.)'
_computing_data_collection       'APEX3 2017.3 (Bruker AXS Inc.)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc.)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'ω-scans and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0088
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            259653
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.636
_diffrn_reflns_theta_min         2.248
_diffrn_source                   'high brilliance microfocus sealed tube '
_exptl_absorpt_coefficient_mu    6.072
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABAS-2016/2
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         7271
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0136
_refine_ls_R_factor_gt           0.0119
_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)+(0.0123P)²+1.8551P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0283
_refine_ls_wR_factor_ref         0.0288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6859
_reflns_number_total             7271
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc04879h2.cif
_cod_data_source_block           DPB_60_0msp_a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1559346
_shelx_shelxl_version_number     2018/1
_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   0.362
_shelx_estimated_absorpt_t_max   0.642
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.74243(2) 0.31710(2) 0.35281(2) 0.00896(2) Uani 1 1 d . . . . .
H0 H 0.6884(15) 0.2622(18) 0.2630(12) 0.021(5) Uiso 1 1 d . . . . .
Cl1 Cl 0.90519(2) 0.22755(3) 0.34330(2) 0.01707(6) Uani 1 1 d . . . . .
N1 N 0.76829(8) 0.47819(10) 0.28678(7) 0.0116(2) Uani 1 1 d . . . . .
N2 N 0.80455(8) 0.37702(10) 0.47625(7) 0.01111(19) Uani 1 1 d . . . . .
C1 C 0.61101(9) 0.40272(12) 0.35396(8) 0.0105(2) Uani 1 1 d . . . . .
C2 C 0.53278(10) 0.36499(12) 0.39423(8) 0.0124(2) Uani 1 1 d . . . . .
H2 H 0.537281 0.288012 0.421230 0.015 Uiso 1 1 calc R U . . .
C3 C 0.44770(10) 0.43763(12) 0.39591(8) 0.0133(2) Uani 1 1 d . . . . .
C4 C 0.43985(10) 0.54837(13) 0.35328(9) 0.0157(2) Uani 1 1 d . . . . .
H4 H 0.381656 0.597665 0.352734 0.019 Uiso 1 1 calc R U . . .
C5 C 0.51615(10) 0.58714(13) 0.31174(9) 0.0146(2) Uani 1 1 d . . . . .
H5 H 0.509567 0.662339 0.282461 0.018 Uiso 1 1 calc R U . . .
C6 C 0.60276(10) 0.51626(12) 0.31264(8) 0.0116(2) Uani 1 1 d . . . . .
C7 C 0.68883(10) 0.55561(12) 0.27459(8) 0.0124(2) Uani 1 1 d . . . . .
C8 C 0.69402(11) 0.66297(13) 0.22966(9) 0.0181(3) Uani 1 1 d . . . . .
H8 H 0.638109 0.717087 0.220373 0.022 Uiso 1 1 calc R U . . .
C9 C 0.78137(12) 0.68993(14) 0.19876(10) 0.0216(3) Uani 1 1 d . . . . .
H9 H 0.785943 0.763085 0.168451 0.026 Uiso 1 1 calc R U . . .
C10 C 0.86205(11) 0.60990(15) 0.21217(9) 0.0197(3) Uani 1 1 d . . . . .
H10 H 0.922459 0.627097 0.191258 0.024 Uiso 1 1 calc R U . . .
C11 C 0.85284(10) 0.50469(14) 0.25653(8) 0.0155(2) Uani 1 1 d . . . . .
H11 H 0.907891 0.449333 0.265983 0.019 Uiso 1 1 calc R U . . .
C12 C 0.36821(10) 0.39880(14) 0.44552(9) 0.0181(3) Uani 1 1 d . . . . .
H12A H 0.302978 0.433771 0.420550 0.027 Uiso 1 1 calc R U . . .
H12B H 0.386604 0.427508 0.503211 0.027 Uiso 1 1 calc R U . . .
H12C H 0.363238 0.309819 0.445126 0.027 Uiso 1 1 calc R U . . .
C21 C 0.70497(10) 0.17583(12) 0.41858(8) 0.0114(2) Uani 1 1 d . . . . .
C22 C 0.65560(11) 0.07084(12) 0.38626(9) 0.0155(2) Uani 1 1 d . . . . .
H22 H 0.643036 0.058758 0.327503 0.019 Uiso 1 1 calc R U . . .
C23 C 0.62399(11) -0.01736(13) 0.43813(10) 0.0186(3) Uani 1 1 d . . . . .
C24 C 0.64201(12) 0.00185(14) 0.52435(10) 0.0207(3) Uani 1 1 d . . . . .
H24 H 0.618140 -0.055546 0.560206 0.025 Uiso 1 1 calc R U . . .
C25 C 0.69440(11) 0.10383(13) 0.55820(9) 0.0176(3) Uani 1 1 d . . . . .
H25 H 0.707922 0.114616 0.617063 0.021 Uiso 1 1 calc R U . . .
C26 C 0.72746(10) 0.19100(12) 0.50594(8) 0.0127(2) Uani 1 1 d . . . . .
C27 C 0.78569(10) 0.29923(12) 0.53669(8) 0.0123(2) Uani 1 1 d . . . . .
C28 C 0.82428(11) 0.32423(13) 0.62038(9) 0.0164(3) Uani 1 1 d . . . . .
H28 H 0.810621 0.270903 0.663159 0.020 Uiso 1 1 calc R U . . .
C29 C 0.88257(11) 0.42735(14) 0.64043(9) 0.0185(3) Uani 1 1 d . . . . .
H29 H 0.909623 0.444641 0.697098 0.022 Uiso 1 1 calc R U . . .
C30 C 0.90144(11) 0.50541(14) 0.57770(9) 0.0174(3) Uani 1 1 d . . . . .
H30 H 0.941543 0.576295 0.590493 0.021 Uiso 1 1 calc R U . . .
C31 C 0.86020(10) 0.47720(13) 0.49586(8) 0.0140(2) Uani 1 1 d . . . . .
H31 H 0.871765 0.530535 0.452411 0.017 Uiso 1 1 calc R U . . .
C32 C 0.57353(14) -0.13163(15) 0.40058(11) 0.0263(3) Uani 1 1 d . . . . .
H32A H 0.534788 -0.113334 0.345280 0.039 Uiso 1 1 calc R U . . .
H32B H 0.527975 -0.162921 0.436819 0.039 Uiso 1 1 calc R U . . .
H32C H 0.624986 -0.192985 0.395211 0.039 Uiso 1 1 calc R U . . .
C91 C 0.95639(17) 0.87624(18) 0.35810(12) 0.0354(4) Uani 1 1 d . . . . .
H91A H 0.956017 0.822056 0.310116 0.053 Uiso 1 1 calc R U . . .
H91B H 1.025659 0.885131 0.388114 0.053 Uiso 1 1 calc R U . . .
H91C H 0.930001 0.956171 0.338517 0.053 Uiso 1 1 calc R U . . .
C92 C 0.89120(14) 0.82309(15) 0.41570(10) 0.0256(3) Uani 1 1 d . . . . .
C93 C 0.88401(14) 0.89457(19) 0.49230(11) 0.0317(4) Uani 1 1 d . . . . .
H93A H 0.867075 0.979232 0.476947 0.048 Uiso 1 1 calc R U . . .
H93B H 0.948930 0.891806 0.530255 0.048 Uiso 1 1 calc R U . . .
H93C H 0.831305 0.859734 0.520152 0.048 Uiso 1 1 calc R U . . .
O94 O 0.84638(15) 0.72806(14) 0.40065(10) 0.0496(4) Uani 1 1 d . . . . .
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'
Cl Cl 0.1484 0.1585 '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'
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
C21 Pt1 C1 93.34(5) . . ?
C21 Pt1 N1 173.53(5) . . ?
C1 Pt1 N1 80.39(5) . . ?
C21 Pt1 N2 80.32(5) . . ?
C1 Pt1 N2 92.98(5) . . ?
N1 Pt1 N2 98.34(4) . . ?
C21 Pt1 Cl1 91.71(4) . . ?
C1 Pt1 Cl1 174.93(4) . . ?
N1 Pt1 Cl1 94.58(3) . . ?
N2 Pt1 Cl1 88.34(3) . . ?
C21 Pt1 H0 94.4(7) . . ?
C1 Pt1 H0 85.5(7) . . ?
N1 Pt1 H0 86.7(7) . . ?
N2 Pt1 H0 174.4(7) . . ?
Cl1 Pt1 H0 93.6(7) . . ?
C11 N1 C7 120.33(12) . . ?
C11 N1 Pt1 125.76(10) . . ?
C7 N1 Pt1 113.89(8) . . ?
C31 N2 C27 120.71(12) . . ?
C31 N2 Pt1 126.13(9) . . ?
C27 N2 Pt1 113.11(9) . . ?
C2 C1 C6 118.80(12) . . ?
C2 C1 Pt1 126.95(10) . . ?
C6 C1 Pt1 114.15(9) . . ?
C1 C2 C3 121.59(12) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 H2 119.2 . . ?
C4 C3 C2 118.81(12) . . ?
C4 C3 C12 120.81(12) . . ?
C2 C3 C12 120.34(13) . . ?
C5 C4 C3 120.63(12) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 120.41(13) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 119.71(12) . . ?
C5 C6 C7 123.07(12) . . ?
C1 C6 C7 117.19(11) . . ?
N1 C7 C8 120.03(12) . . ?
N1 C7 C6 114.32(11) . . ?
C8 C7 C6 125.64(12) . . ?
C9 C8 C7 119.39(14) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C10 119.76(13) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C10 C9 118.56(13) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
N1 C11 C10 121.92(13) . . ?
N1 C11 H11 119.0 . . ?
C10 C11 H11 119.0 . . ?
C3 C12 H12A 109.5 . . ?
C3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C22 C21 C26 119.10(12) . . ?
C22 C21 Pt1 126.24(10) . . ?
C26 C21 Pt1 114.57(9) . . ?
C21 C22 C23 121.54(13) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 H22 119.2 . . ?
C24 C23 C22 118.75(13) . . ?
C24 C23 C32 121.48(14) . . ?
C22 C23 C32 119.75(14) . . ?
C25 C24 C23 120.69(13) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C24 C25 C26 120.27(13) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C21 119.52(13) . . ?
C25 C26 C27 123.68(12) . . ?
C21 C26 C27 116.80(12) . . ?
N2 C27 C28 119.70(13) . . ?
N2 C27 C26 114.78(12) . . ?
C28 C27 C26 125.48(12) . . ?
C29 C28 C27 119.46(13) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C28 C29 C30 119.96(13) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C31 C30 C29 118.22(13) . . ?
C31 C30 H30 120.9 . . ?
C29 C30 H30 120.9 . . ?
N2 C31 C30 121.94(13) . . ?
N2 C31 H31 119.0 . . ?
C30 C31 H31 119.0 . . ?
C23 C32 H32A 109.5 . . ?
C23 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C23 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C92 C91 H91A 109.5 . . ?
C92 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C92 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
O94 C92 C93 121.63(18) . . ?
O94 C92 C91 122.14(17) . . ?
C93 C92 C91 116.22(16) . . ?
C92 C93 H93A 109.5 . . ?
C92 C93 H93B 109.5 . . ?
H93A C93 H93B 109.5 . . ?
C92 C93 H93C 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 109.5 . . ?
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 C21 1.9962(13) . ?
Pt1 C1 2.0035(12) . ?
Pt1 N1 2.1283(11) . ?
Pt1 N2 2.1414(11) . ?
Pt1 Cl1 2.4264(3) . ?
Pt1 H0 1.63(2) . ?
N1 C11 1.3433(17) . ?
N1 C7 1.3533(17) . ?
N2 C31 1.3386(17) . ?
N2 C27 1.3572(17) . ?
C1 C2 1.3913(17) . ?
C1 C6 1.4121(18) . ?
C2 C3 1.3982(18) . ?
C2 H2 0.9500 . ?
C3 C4 1.395(2) . ?
C3 C12 1.5039(19) . ?
C4 C5 1.3858(19) . ?
C4 H4 0.9500 . ?
C5 C6 1.3983(18) . ?
C5 H5 0.9500 . ?
C6 C7 1.4652(18) . ?
C7 C8 1.3950(19) . ?
C8 C9 1.384(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.384(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.379(2) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C21 C22 1.3889(18) . ?
C21 C26 1.4098(18) . ?
C22 C23 1.396(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.396(2) . ?
C23 C32 1.506(2) . ?
C24 C25 1.387(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.4007(19) . ?
C25 H25 0.9500 . ?
C26 C27 1.4642(19) . ?
C27 C28 1.3980(18) . ?
C28 C29 1.385(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.387(2) . ?
C29 H29 0.9500 . ?
C30 C31 1.3861(19) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C91 C92 1.503(3) . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?
C92 O94 1.210(2) . ?
C92 C93 1.488(2) . ?
C93 H93A 0.9800 . ?
C93 H93B 0.9800 . ?
C93 H93C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C10 H10 Cl1 0.95 2.71 3.6345(15) 165.2 2_755 yes
C11 H11 Cl1 0.95 2.74 3.3795(15) 124.9 . yes
C31 H31 O94 0.95 2.33 3.151(2) 144.1 . yes
