Platinum(ii) alkyl complexes of chelating dibridgehead diphosphines P((CH2)n)3P (n = 14, 18, 22); facile cis/trans isomerizations interconverting gyroscope and parachute like adducts
Zhu, Yun; Ehnbom, Andreas; Fiedler, Tobias; Shu, Yi; Bhuvanesh, Nattamai; Hall, Michael B.; Gladysz, John A.; Dalton Transactions  (2021) –; doi:10.1039/D1DT02321G

data_7708168
_publ_section_title
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 Platinum(ii) alkyl complexes of chelating dibridgehead diphosphines
 P((CH2)n)3P (n = 14, 18, 22); facile cis/trans isomerizations
 interconverting gyroscope and parachute like adducts
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02321G
_journal_year                    2021
_chemical_formula_moiety         'C43 H87 Cl P2 Pt'
_chemical_formula_sum            'C43 H87 Cl P2 Pt'
_chemical_formula_weight         896.60
_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     dual
_audit_creation_date             2020-09-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
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_audit_update_record
;
2021-08-20 deposited with the CCDC.	2021-08-23 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90.909(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2658(9)
_cell_length_b                   13.6513(8)
_cell_length_c                   19.9653(11)
_cell_measurement_reflns_used    9483
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      27.476
_cell_measurement_theta_min      2.836
_cell_volume                     4432.7(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker APEX3 (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker QUEST PHOTON-II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            173120
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         1.948
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.325
_exptl_absorpt_correction_T_max  0.2616
_exptl_absorpt_correction_T_min  0.0906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1310 before and 0.0653 after correction.
The Ratio of minimum to maximum transmission is 0.3463.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.493
_exptl_crystal_size_mid          0.475
_exptl_crystal_size_min          0.292
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.00051(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         10146
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0183
_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/[\s^2^(Fo^2^)+(0.0129P)^2^+4.2853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0387
_refine_ls_wR_factor_ref         0.0402
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9307
_reflns_number_total             10146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02321g3.cif
_cod_data_source_block           cis14ptmecl
_cod_database_code               7708168
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.444
_shelx_estimated_absorpt_t_min   0.291
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Pt1-Cl1 \\sim Pt1-Cl1A
 with sigma of 0.02
 Pt1-C1A \\sim Pt1-C1
 with sigma of 0.02
 C39A-C38 \\sim C39-C38 \\sim C40-C41 \\sim C40A-C41
 with sigma of 0.01
 C39-C40 \\sim C40A-C39A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C41 \\sim C40 \\sim C38 \\sim C39 \\sim C39A \\sim C40A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
Pt1 \\sim Cl1 \\sim C1 \\sim Cl1A \\sim C1A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(C1) = Uanis(C1A)
4. Rigid body (RIGU) restrains
 C41, C40, C38, C39, C39A, C40A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Pt1, Cl1, C1, Cl1A, C1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(Cl1A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(Cl1)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=FVAR(1)
 Sof(H41C)=Sof(H41D)=Sof(H38C)=Sof(H38D)=Sof(C39A)=Sof(H39C)=Sof(H39D)=
 Sof(C40A)=Sof(H40C)=Sof(H40D)=1-FVAR(2)
 Sof(H41A)=Sof(H41B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H38A)=Sof(H38B)=Sof(C39)=
 Sof(H39A)=Sof(H39B)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C43(H43A,H43B), C2(H2A,H2B), C30(H30A,H30B), C13(H13A,H13B),
 C29(H29A,H29B), C12(H12A,H12B), C16(H16A,H16B), C15(H15A,H15B), C42(H42A,H42B),
  C31(H31A,H31B), C27(H27A,H27B), C32(H32A,H32B), C11(H11A,H11B), C33(H33A,
 H33B), C17(H17A,H17B), C28(H28A,H28B), C3(H3A,H3B), C25(H25A,H25B), C26(H26A,
 H26B), C9(H9A,H9B), C34(H34A,H34B), C6(H6A,H6B), C41(H41A,H41B), C41(H41C,
 H41D), C18(H18A,H18B), C7(H7A,H7B), C10(H10A,H10B), C4(H4A,H4B), C24(H24A,
 H24B), C5(H5A,H5B), C8(H8A,H8B), C36(H36A,H36B), C23(H23A,H23B), C35(H35A,
 H35B), C19(H19A,H19B), C21(H21A,H21B), C40(H40A,H40B), C38(H38A,H38B),
 C38(H38C,H38D), C20(H20A,H20B), C22(H22A,H22B), C39(H39A,H39B), C37(H37A,H37B),
  C39A(H39C,H39D), C40A(H40C,H40D)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC)
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_shelx_res_checksum              15567
_olex2_submission_special_instructions 'No special instructions were received'