#------------------------------------------------------------------------------
#$Date: 2020-10-14 03:59:47 +0300 (Wed, 14 Oct 2020) $
#$Revision: 258351 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/93/1559353.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_1559353
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            'C32 H27 Cl N2 Pt'
_chemical_formula_weight         670.09
_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   geom
_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                 106.456(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8828(7)
_cell_length_b                   16.0961(9)
_cell_length_c                   13.7671(7)
_cell_measurement_reflns_used    9207
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.18
_cell_volume                     2525.3(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 0.999
_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  0.0394
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            89295
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.585
_diffrn_reflns_theta_min         1.787
_diffrn_source                   'high brilliance microfocus sealed tube '
_exptl_absorpt_coefficient_mu    5.687
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.000
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         7745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0182
_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)+(0.0167P)²+3.2229P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0408
_refine_ls_wR_factor_ref         0.0422
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6945
_reflns_number_total             7745
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc04879h2.cif
_cod_data_source_block           DPC78b_0msp_a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1559353
_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   0.368
_shelx_estimated_absorpt_t_max   0.659
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 0.28757(2) 0.45270(2) 0.67470(2) 0.01069(2) Uani 1 1 d . . . . .
Cl1 Cl 0.41758(5) 0.56917(3) 0.73686(4) 0.01946(10) Uani 1 1 d . . . . .
N1 N 0.31278(15) 0.39558(11) 0.81933(12) 0.0138(3) Uani 1 1 d . . . . .
N2 N 0.43069(15) 0.38533(10) 0.64785(13) 0.0151(3) Uani 1 1 d . . . . .
C1 C 0.18438(17) 0.35248(13) 0.63331(15) 0.0149(4) Uani 1 1 d . . . . .
C2 C 0.10993(19) 0.33624(15) 0.53692(16) 0.0212(4) Uani 1 1 d . . . . .
H2 H 0.105015 0.374935 0.483774 0.025 Uiso 1 1 calc R U . . .
C3 C 0.0426(2) 0.26386(17) 0.51762(18) 0.0282(5) Uani 1 1 d . . . . .
C4 C 0.0522(2) 0.20701(16) 0.5955(2) 0.0306(6) Uani 1 1 d . . . . .
H4 H 0.009068 0.156557 0.582260 0.037 Uiso 1 1 calc R U . . .
C5 C 0.1238(2) 0.22285(15) 0.69233(18) 0.0250(5) Uani 1 1 d . . . . .
H5 H 0.128930 0.183465 0.744800 0.030 Uiso 1 1 calc R U . . .
C6 C 0.18851(18) 0.29657(13) 0.71303(15) 0.0165(4) Uani 1 1 d . . . . .
C7 C 0.25719(18) 0.32168(13) 0.81498(15) 0.0151(4) Uani 1 1 d . . . . .
C8 C 0.2656(2) 0.27709(14) 0.90312(17) 0.0214(4) Uani 1 1 d . . . . .
H8 H 0.225924 0.225506 0.900230 0.026 Uiso 1 1 calc R U . . .
C9 C 0.3320(2) 0.30824(15) 0.99509(17) 0.0241(5) Uani 1 1 d . . . . .
H9 H 0.336275 0.279088 1.056029 0.029 Uiso 1 1 calc R U . . .
C10 C 0.3920(2) 0.38194(15) 0.99773(16) 0.0232(5) Uani 1 1 d . . . . .
H10 H 0.440185 0.403321 1.059967 0.028 Uiso 1 1 calc R U . . .
C11 C 0.38053(19) 0.42399(14) 0.90808(16) 0.0193(4) Uani 1 1 d . . . . .
H11 H 0.421980 0.474631 0.909378 0.023 Uiso 1 1 calc R U . . .
C12 C -0.0392(3) 0.2482(2) 0.4135(2) 0.0422(7) Uani 1 1 d . . . . .
H12A H -0.070385 0.301253 0.382317 0.063 Uiso 1 1 calc R U . . .
H12B H -0.104101 0.212728 0.419031 0.063 Uiso 1 1 calc R U . . .
H12C H 0.003787 0.220526 0.371562 0.063 Uiso 1 1 calc R U . . .
C21 C 0.27211(17) 0.48920(13) 0.53193(14) 0.0143(4) Uani 1 1 d . . . . .
C22 C 0.19569(19) 0.54798(15) 0.47501(16) 0.0211(4) Uani 1 1 d . . . . .
H22 H 0.145508 0.577956 0.505263 0.025 Uiso 1 1 calc R U . . .
C23 C 0.1911(2) 0.56396(17) 0.37387(18) 0.0271(5) Uani 1 1 d . . . . .
C24 C 0.2631(2) 0.51797(18) 0.32997(17) 0.0284(5) Uani 1 1 d . . . . .
H24 H 0.256843 0.525418 0.260186 0.034 Uiso 1 1 calc R U . . .
C25 C 0.3429(2) 0.46210(15) 0.38552(17) 0.0237(5) Uani 1 1 d . . . . .
H25 H 0.393389 0.432962 0.354827 0.028 Uiso 1 1 calc R U . . .
C26 C 0.34996(18) 0.44796(13) 0.48764(16) 0.0163(4) Uani 1 1 d . . . . .
C27 C 0.43689(19) 0.39271(13) 0.55142(16) 0.0168(4) Uani 1 1 d . . . . .
C28 C 0.5221(2) 0.34860(14) 0.52018(19) 0.0241(5) Uani 1 1 d . . . . .
H28 H 0.528448 0.355087 0.453332 0.029 Uiso 1 1 calc R U . . .
C29 C 0.5968(2) 0.29568(15) 0.5872(2) 0.0300(5) Uani 1 1 d . . . . .
H29 H 0.653593 0.264356 0.566333 0.036 Uiso 1 1 calc R U . . .
C30 C 0.5885(2) 0.28843(15) 0.6855(2) 0.0270(5) Uani 1 1 d . . . . .
H30 H 0.639513 0.252416 0.732729 0.032 Uiso 1 1 calc R U . . .
C31 C 0.50494(19) 0.33446(13) 0.71319(18) 0.0203(4) Uani 1 1 d . . . . .
H31 H 0.499535 0.330162 0.780542 0.024 Uiso 1 1 calc R U . . .
C32 C 0.1126(2) 0.6302(2) 0.3145(2) 0.0406(7) Uani 1 1 d . . . . .
H32A H 0.131726 0.639746 0.250710 0.061 Uiso 1 1 calc R U . . .
H32B H 0.124075 0.681794 0.353985 0.061 Uiso 1 1 calc R U . . .
H32C H 0.030591 0.612517 0.300079 0.061 Uiso 1 1 calc R U . . .
C41 C 0.13563(19) 0.50830(14) 0.67667(17) 0.0191(4) Uani 1 1 d . . . . .
H41 H 0.083000 0.515905 0.611026 0.023 Uiso 1 1 calc R U . . .
C42 C 0.0937(2) 0.53650(14) 0.75040(18) 0.0236(5) Uani 1 1 d . . . . .
H42 H 0.014075 0.553910 0.730074 0.028 Uiso 1 1 calc R U . . .
C43 C 0.1545(2) 0.54437(14) 0.85972(18) 0.0233(5) Uani 1 1 d . . . . .
C44 C 0.1213(2) 0.49759(16) 0.93209(19) 0.0270(5) Uani 1 1 d . . . . .
H44 H 0.059710 0.458048 0.912115 0.032 Uiso 1 1 calc R U . . .
C45 C 0.1792(3) 0.50939(19) 1.0334(2) 0.0374(7) Uani 1 1 d . . . . .
H45 H 0.158891 0.477661 1.084116 0.045 Uiso 1 1 calc R U . . .
C46 C 0.2666(3) 0.5680(2) 1.0591(2) 0.0468(8) Uani 1 1 d . . . . .
H46 H 0.306709 0.575143 1.128776 0.056 Uiso 1 1 calc R U . . .
C47 C 0.2984(3) 0.61510(17) 0.99251(19) 0.0352(7) Uani 1 1 d . . . . .
H47 H 0.358072 0.655970 1.013317 0.042 Uiso 1 1 calc R U . . .
C48 C 0.2426(3) 0.60253(16) 0.8946(2) 0.0343(6) Uani 1 1 d . . . . .
H48 H 0.264924 0.635570 0.845930 0.041 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'
Cl Cl 0.1484 0.1585 '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'
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
C1 Pt1 C21 94.47(8) . . ?
C1 Pt1 C41 83.32(9) . . ?
C21 Pt1 C41 92.81(8) . . ?
C1 Pt1 N2 89.72(7) . . ?
C21 Pt1 N2 80.55(7) . . ?
C41 Pt1 N2 170.01(8) . . ?
C1 Pt1 N1 80.33(7) . . ?
C21 Pt1 N1 170.96(7) . . ?
C41 Pt1 N1 93.90(8) . . ?
N2 Pt1 N1 91.98(7) . . ?
C1 Pt1 Cl1 175.81(6) . . ?
C21 Pt1 Cl1 89.53(6) . . ?
C41 Pt1 Cl1 97.76(7) . . ?
N2 Pt1 Cl1 89.69(5) . . ?
N1 Pt1 Cl1 95.55(5) . . ?
C11 N1 C7 120.01(18) . . ?
C11 N1 Pt1 126.37(14) . . ?
C7 N1 Pt1 113.52(13) . . ?
C31 N2 C27 120.07(18) . . ?
C31 N2 Pt1 126.66(14) . . ?
C27 N2 Pt1 113.08(14) . . ?
C2 C1 C6 119.59(19) . . ?
C2 C1 Pt1 126.29(16) . . ?
C6 C1 Pt1 114.08(14) . . ?
C1 C2 C3 120.8(2) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
C4 C3 C2 119.0(2) . . ?
C4 C3 C12 120.9(2) . . ?
C2 C3 C12 120.1(2) . . ?
C5 C4 C3 121.0(2) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 120.3(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 119.1(2) . . ?
C5 C6 C7 123.6(2) . . ?
C1 C6 C7 117.16(18) . . ?
N1 C7 C8 120.13(19) . . ?
N1 C7 C6 114.64(17) . . ?
C8 C7 C6 125.20(19) . . ?
C9 C8 C7 119.6(2) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C10 C9 C8 119.5(2) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 C11 118.6(2) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
N1 C11 C10 122.0(2) . . ?
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 118.74(18) . . ?
C22 C21 Pt1 127.94(16) . . ?
C26 C21 Pt1 113.33(15) . . ?
C21 C22 C23 121.4(2) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C24 C23 C22 118.5(2) . . ?
C24 C23 C32 120.4(2) . . ?
C22 C23 C32 121.0(2) . . ?
C25 C24 C23 121.3(2) . . ?
C25 C24 H24 119.4 . . ?
C23 C24 H24 119.4 . . ?
C24 C25 C26 120.1(2) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C21 119.8(2) . . ?
C25 C26 C27 122.3(2) . . ?
C21 C26 C27 117.89(18) . . ?
N2 C27 C28 120.1(2) . . ?
N2 C27 C26 114.74(18) . . ?
C28 C27 C26 125.2(2) . . ?
C29 C28 C27 119.5(2) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C28 C29 C30 119.6(2) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
C31 C30 C29 118.7(2) . . ?
C31 C30 H30 120.7 . . ?
C29 C30 H30 120.7 . . ?
N2 C31 C30 122.1(2) . . ?
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 . . ?
C42 C41 Pt1 133.60(18) . . ?
C42 C41 H41 113.2 . . ?
Pt1 C41 H41 113.2 . . ?
C41 C42 C43 128.7(2) . . ?
C41 C42 H42 115.6 . . ?
C43 C42 H42 115.6 . . ?
C48 C43 C44 117.2(2) . . ?
C48 C43 C42 120.9(2) . . ?
C44 C43 C42 121.8(2) . . ?
C45 C44 C43 119.1(2) . . ?
C45 C44 H44 120.4 . . ?
C43 C44 H44 120.4 . . ?
C46 C45 C44 118.6(2) . . ?
C46 C45 H45 120.7 . . ?
C44 C45 H45 120.7 . . ?
C47 C46 C45 123.9(3) . . ?
C47 C46 H46 118.0 . . ?
C45 C46 H46 118.0 . . ?
C46 C47 C48 117.0(2) . . ?
C46 C47 H47 121.5 . . ?
C48 C47 H47 121.5 . . ?
C47 C48 C43 124.1(2) . . ?
C47 C48 H48 117.9 . . ?
C43 C48 H48 117.9 . . ?
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 C1 2.009(2) . ?
Pt1 C21 2.0094(19) . ?
Pt1 C41 2.022(2) . ?
Pt1 N2 2.1357(17) . ?
Pt1 N1 2.1358(16) . ?
Pt1 Cl1 2.4258(5) . ?
N1 C11 1.339(3) . ?
N1 C7 1.354(3) . ?
N2 C31 1.345(3) . ?
N2 C27 1.355(3) . ?
C1 C2 1.395(3) . ?
C1 C6 1.409(3) . ?
C2 C3 1.396(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(4) . ?
C3 C12 1.507(3) . ?
C4 C5 1.387(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.399(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.466(3) . ?
C7 C8 1.389(3) . ?
C8 C9 1.382(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.379(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.380(3) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C21 C22 1.389(3) . ?
C21 C26 1.410(3) . ?
C22 C23 1.402(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.392(4) . ?
C23 C32 1.498(4) . ?
C24 C25 1.372(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.403(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.454(3) . ?
C27 C28 1.401(3) . ?
C28 C29 1.379(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.389(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.376(3) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C41 C42 1.331(3) . ?
C41 H41 0.9500 . ?
C42 C43 1.479(3) . ?
C42 H42 0.9500 . ?
C43 C48 1.385(4) . ?
C43 C44 1.392(3) . ?
C44 C45 1.382(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.373(4) . ?
C45 H45 0.9500 . ?
C46 C47 1.324(4) . ?
C46 H46 0.9500 . ?
C47 C48 1.338(4) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
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 2.86 3.796(2) 167.2 3_667 yes
