Bi- and tridentate stannylphosphines and their coordination to low-valent platinum.
Salazar-Díaz, J Jacobo; Muñoz-Hernández, Miguel A; Rufino-Felipe, Ernesto; Flores-Alamo, Marcos; Ramírez-Solís, Alejandro; Montiel-Palma, Virginia; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15896–15905; doi:10.1039/c9dt03317c

data_7701202
_publ_section_title
;
 Bi- and tridentate stannylphosphines and their coordination to low-valent
 platinum.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15896
_journal_page_last               15905
_journal_paper_doi               10.1039/c9dt03317c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C40 H40 P2 Pt Sn'
_chemical_formula_sum            'C40 H40 P2 Pt Sn'
_chemical_formula_weight         896.44
_chemical_properties_physical    Air-sensitive
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2019-04-13 deposited with the CCDC.    2019-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.936(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.9322(2)
_cell_length_b                   28.0658(3)
_cell_length_c                   28.8753(6)
_cell_measurement_reflns_used    18519
_cell_measurement_temperature    99.99(11)
_cell_measurement_theta_max      29.1170
_cell_measurement_theta_min      2.7180
_cell_volume                     6904.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1539
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     54.00  87.00   0.75   15.59    --   15.24-178.00 -30.00   44
  2  \w     -3.00  83.25   0.75   15.59    --   15.24  38.00  30.00  115
  3  \w    -32.00  80.50   0.75   15.59    --   15.24   0.00 120.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0289326000
_diffrn_orient_matrix_UB_12      -0.0149144000
_diffrn_orient_matrix_UB_13      0.0230299000
_diffrn_orient_matrix_UB_21      -0.0744779000
_diffrn_orient_matrix_UB_22      -0.0111527000
_diffrn_orient_matrix_UB_23      -0.0114573000
_diffrn_orient_matrix_UB_31      0.0233855000
_diffrn_orient_matrix_UB_32      -0.0170892000
_diffrn_orient_matrix_UB_33      -0.0125834000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            35608
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.184
_diffrn_reflns_theta_min         2.546
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.892
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       prism
_exptl_crystal_F_000             3504
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.660
_refine_diff_density_min         -1.363
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         15653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.4190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13708
_reflns_number_total             15653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03317c2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7701201--7701206.cif.'
_cod_database_code               7701202
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H P Sn Pt'
_reflns_odcompleteness_completeness 97.01
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C47(H47A,H47B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C43(H43), C44(H44),
  C45(H45), C46(H46), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53),
 C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C61(H61), C62(H62), C63(H63),
  C64(H64), C65(H65), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71),
 C73(H73), C74(H74), C75(H75), C76(H76), C77(H77)
2.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C78(H78A,H78B,
 H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C)
;
_shelx_res_checksum              79753
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.864
_oxdiff_exptl_absorpt_empirical_full_min 0.613