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_7701205
_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         'C50 H42 P2 Sn'
_chemical_formula_sum            'C50 H42 P2 Sn'
_chemical_formula_weight         823.46
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-13 deposited with the CCDC.    2019-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                100.250(5)
_cell_angle_beta                 103.764(6)
_cell_angle_gamma                92.688(4)
_cell_formula_units_Z            2
_cell_length_a                   11.0985(7)
_cell_length_b                   11.5385(5)
_cell_length_c                   16.3580(11)
_cell_measurement_reflns_used    6485
_cell_measurement_temperature    100.46(10)
_cell_measurement_theta_max      27.5670
_cell_measurement_theta_min      2.8150
_cell_volume                     1993.4(2)
_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, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100.46(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1539
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega    2.00   51.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2374   57.0000 -180.0000 49

  2 omega  -52.00   32.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -57.0000 -180.0000 84

  3 omega    1.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2374   19.0000    0.0000 86

  4 omega  -11.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2374   77.0000   60.0000 94

  5 omega   25.00   76.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2374   38.0000 -150.0000 51

  6 omega  -51.00   32.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -57.0000   30.0000 83

  7 omega  -51.00   32.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -57.0000  -90.0000 83

  8 omega  -11.00   54.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2374   77.0000  -90.0000 65

  9 omega  -71.00  -26.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0187  127.0000   -2.1060 45

 10 omega  -74.00  -27.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0187  132.0000  102.4713 47

 11 omega  -72.00  -27.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0187  129.0000 -118.4049 45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0283948000
_diffrn_orient_matrix_UB_12      -0.0202686000
_diffrn_orient_matrix_UB_13      0.0300378000
_diffrn_orient_matrix_UB_21      -0.0580210000
_diffrn_orient_matrix_UB_22      -0.0108014000
_diffrn_orient_matrix_UB_23      -0.0311068000
_diffrn_orient_matrix_UB_31      0.0139596000
_diffrn_orient_matrix_UB_32      -0.0583887000
_diffrn_orient_matrix_UB_33      -0.0142055000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1509
_diffrn_reflns_av_unetI/netI     0.1127
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25938
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.614
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.756
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.860
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_F_000             844
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.2494
_exptl_crystal_size_mid          0.1202
_exptl_crystal_size_min          0.0677
_refine_diff_density_max         3.176
_refine_diff_density_min         -1.539
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         7012
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1047P)^2^+0.9506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1824
_refine_ls_wR_factor_ref         0.1987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5601
_reflns_number_total             7012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03317c2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7701201--7701206.cif.'
_cod_database_code               7701205
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C50 H42 P2 Sn'
_reflns_odcompleteness_completeness 99.94
_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
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.05
and sigma for terminal atoms of 0.1
3. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C38(H38A,H38B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), 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), C40(H40), C41(H41), C42(H42), C43(H43),
  C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50)
;
_shelx_res_checksum              8947
_olex2_date_sample_data_collection 2016-03-18
_olex2_submission_special_instructions 'No special instructions were received'