Mononuclear palladium(ii) and platinum(ii) complexes of P,C-donor ligands: synthesis, crystal structures, cytotoxicity, and mechanistic studies of a highly stereoselective Mizoroki‒Heck reaction
Sabounchei, Seyyed Javad; Hosseinzadeh, Marjan; Salehzadeh, Sadegh; Maleki, Farahnaz; Gable, Robert W.; Inorganic Chemistry Frontiers 4 (2017) 2107–; doi:10.1039/C7QI00568G

data_4349784
_publ_section_title
;
 Mononuclear palladium(ii) and platinum(ii) complexes of P,C-donor
 ligands: synthesis, crystal structures, cytotoxicity, and mechanistic
 studies of a highly stereoselective Mizoroki--Heck reaction
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              2107
_journal_paper_doi               10.1039/C7QI00568G
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         'C33 H27 Cl2 N O3 P2 Pt'
_chemical_formula_sum            'C33 H27 Cl2 N O3 P2 Pt'
_chemical_formula_weight         813.48
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-01
_audit_creation_method
;

Olex2 1.2

(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)

;
_audit_update_record
;
2015-10-17 deposited with the CCDC.
2017-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.764(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3504(2)
_cell_length_b                   17.9198(2)
_cell_length_c                   14.0028(2)
_cell_measurement_reflns_used    21866
_cell_measurement_temperature    130.00(10)
_cell_measurement_theta_max      30.4960
_cell_measurement_theta_min      3.7110
_cell_volume                     3016.97(9)
_computing_cell_refinement
;

CrysAlisPro, Agilent Technologies,

Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)

(compiled Aug 13 2014,18:06:01)

;
_computing_data_collection
;

CrysAlisPro, Agilent Technologies,

Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)

(compiled Aug 13 2014,18:06:01)

;
_computing_data_reduction
;

CrysAlisPro, Agilent Technologies,

Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)

(compiled Aug 13 2014,18:06:01)

;
_computing_molecular_graphics    'Olex2(Dolomanov et al., 2009)'
_computing_publication_material  'Olex2(Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL(Sheldrick, 2008)'
_computing_structure_solution    'ShelXT(Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_details
;

  1 omega   -2.00  
23.00   1.0000   10.0000

omega____ theta____ kappa____ phi______ frames

    -     
 13.4921  -37.0000 -120.0000 25

  2 omega 
-32.00   -3.00   1.0000  
10.0000

omega____ theta____ kappa____ phi______ frames

    -     
-13.7265   77.0000 -180.0000
29

  3 omega   37.00  
62.00   1.0000   10.0000

omega____ theta____ kappa____ phi______ frames

    -     
-13.7265   77.0000 -180.0000
25

  4 omega 
-77.00  -51.00   1.0000  
10.0000

omega____ theta____ kappa____ phi______ frames

    -     
-13.7265  -37.0000   90.0000 26

  5 omega 
-74.00  101.00   1.0000  
10.0000

omega____ theta____ kappa____ phi______ frames

    -       13.4921    0.0000 
120.0000 175

  6 omega   12.00  
52.00   1.0000   10.0000

omega____ theta____ kappa____ phi______ frames

    -       13.4921 
-99.0000  150.0000 40

  7 omega 
-20.00   27.00   1.0000  
10.0000

omega____ theta____ kappa____ phi______ frames

    -     
-13.7265  -99.0000  120.0000 47

  8 omega    3.00  
28.00   1.0000   10.0000

omega____ theta____ kappa____ phi______ frames

    -       13.4921  
37.0000  150.0000 25

  9 omega 
-97.00  -62.00   1.0000  
10.0000

omega____ theta____ kappa____ phi______ frames

    -     
-13.7265  178.0000  -90.0000 35

 10 omega -101.00  -69.00  
1.0000   10.0000

omega____ theta____ kappa____ phi______ frames

    -     
-13.7265  178.0000 -180.0000
32

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0332781000
_diffrn_orient_matrix_UB_12      0.0154766000
_diffrn_orient_matrix_UB_13      0.0230414000
_diffrn_orient_matrix_UB_21      -0.0209264000
_diffrn_orient_matrix_UB_22      0.0269398000
_diffrn_orient_matrix_UB_23      -0.0411702000
_diffrn_orient_matrix_UB_31      -0.0439813000
_diffrn_orient_matrix_UB_32      -0.0245191000
_diffrn_orient_matrix_UB_33      -0.0306358000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37519
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.771
_diffrn_reflns_theta_min         2.803
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.970
_exptl_absorpt_correction_T_max  0.583
_exptl_absorpt_correction_T_min  0.256
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;

CrysAlisPro, Agilent Technologies,

Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)

(compiled Aug 13 2014,18:06:01)

Numerical absorption correction based on gaussian integration over

                  a multifaceted crystal
model

Empirical absorption correction using spherical harmonics,

 implemented in SCALE3 ABSPACK scaling
algorithm.

;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_description       needle
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.3649
_exptl_crystal_size_mid          0.1741
_exptl_crystal_size_min          0.1247
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         8653
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0209
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0138P)^2^+1.0498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0422
_refine_ls_wR_factor_ref         0.0448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7916
_reflns_number_total             8653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qi00568g2.cif
_cod_data_source_block           rwg_2015_9gau
_cod_original_cell_volume        3016.96(8)
_cod_database_code               4349784
_chemical_oxdiff_formula         'C33 H27 Cl2 N O3 P3 Pt'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;

1. Fixed Uiso

 At 1.2 times of:

  All C(H) groups, All C(H,H)
groups

2. Uiso/Uaniso restraints and constraints

Uanis(O3) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of
0.006

3.a Ternary CH refined with riding coordinates:

 C1(H1)

3.b Secondary CH2 refined with riding coordinates:

 C21(H21A,H21B)

3.c Aromatic/amide H refined with riding coordinates:

 C4(H4), C6(H6), C7(H7), C8(H8),
C10(H10), C11(H11), C12(H12), C13(H13),

 C14(H14), C16(H16), C17(H17), C18(H18),
C19(H19), C20(H20), C23(H23), C24(H24),

  C25(H25), C26(H26), C27(H27), C29(H29),
C30(H30), C31(H31), C32(H32), C33(H33)

;
_shelx_res_checksum              3024
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'