Fluorination and hydrolytic stability of water-soluble platinum complexes with a borane-bridged diphosphoramidite ligand
Culpepper, Johnathan D.; Lee, Kyounghoon; Portis, William; Swenson, Dale C.; Daly, Scott R.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01482C

data_7710943
_publ_section_title
;
 Fluorination and hydrolytic stability of water-soluble platinum complexes
 with a borane-bridged diphosphoramidite ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01482C
_journal_year                    2022
_chemical_formula_moiety
'2(C18 H41 B Cl2 F N3 O4 P2 Pt), Cl, C4 H10 O, C18 H36 K N2 O6'
_chemical_formula_sum            'C58 H128 B2 Cl5 F2 K N8 O15 P4 Pt2'
_chemical_formula_weight         1967.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-05-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-12 deposited with the CCDC.	2022-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.243(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   84.172(8)
_cell_length_b                   10.5703(11)
_cell_length_c                   19.8514(19)
_cell_measurement_reflns_used    9606
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.385
_cell_measurement_theta_min      2.2925
_cell_volume                     17193(3)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture Duo Photon 3'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       104
_diffrn_reflns_limit_h_min       -104
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            111211
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.407
_diffrn_reflns_theta_min         1.943
_exptl_absorpt_coefficient_mu    3.592
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1164 before and 0.0928 after correction.
The Ratio of minimum to maximum transmission is 0.7310.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       irregular
_exptl_crystal_F_000             8000
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.085
_refine_diff_density_max         1.404
_refine_diff_density_min         -1.725
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1129
_refine_ls_number_reflns         17567
_refine_ls_number_restraints     1484
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0478
_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^)+287.8160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16202
_reflns_number_total             17567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01482c2.cif
_cod_data_source_block           dal2045
_cod_database_code               7710943
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.750
_shelx_estimated_absorpt_t_min   0.455
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N41 \\sim N42 \\sim C41 \\sim C42 \\sim O43 \\sim C44 \\sim C45 \\sim O46 \\sim
C47 \\sim C48 \\sim C51 \\sim C52 \\sim O53 \\sim C54 \\sim C55 \\sim O56 \\sim
C57 \\sim C58 \\sim C61 \\sim C62 \\sim O63 \\sim C64 \\sim C65 \\sim O66 \\sim
C67 \\sim C68 \\sim N41A \\sim N42A \\sim C41A \\sim C42A \\sim O43A \\sim C44A
\\sim C45A \\sim O46A \\sim C47A \\sim C48A \\sim C51A \\sim C52A \\sim O53A
\\sim C54A \\sim C55A \\sim O56A \\sim C57A \\sim C58A \\sim C61A \\sim C62A
\\sim O63A \\sim C64A \\sim C65A \\sim O66A \\sim C67A \\sim C68A: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 O9, C37, C38, C39, C40, K1, N41, N42, C41, C42, O43, C44, C45, O46, C47, C48,
 C51, C52, O53, C54, C55, O56, C57, C58, C61, C62, O63, C64, C65, O66, C67, C68,
  N41A, N42A, C41A, C42A, O43A, C44A, C45A, O46A, C47A, C48A, C51A, C52A, O53A,
 C54A, C55A, O56A, C57A, C58A, C61A, C62A, O63A, C64A, C65A, O66A, C67A, C68A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{N41, N42, C41, C42, O43, C44, C45, O46, C47, C48, C51, C52, O53, C54, C55,
O56, C57, C58, C61, C62, O63, C64, C65, O66, C67, C68} sigma for 1-2: 0.005,
1-3: 0.005
as
{N41A, N42A, C41A, C42A, O43A, C44A, C45A, O46A, C47A, C48A, C51A, C52A, O53A,
C54A, C55A, O56A, C57A, C58A, C61A, C62A, O63A, C64A, C65A, O66A, C67A, C68A}
5. Others
 Sof(N41A)=Sof(N42A)=Sof(C41A)=Sof(H41C)=Sof(H41D)=Sof(C42A)=Sof(H42C)=
 Sof(H42D)=Sof(O43A)=Sof(C44A)=Sof(H44C)=Sof(H44D)=Sof(C45A)=Sof(H45C)=
 Sof(H45D)=Sof(O46A)=Sof(C47A)=Sof(H47C)=Sof(H47D)=Sof(C48A)=Sof(H48C)=
 Sof(H48D)=Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(C52A)=Sof(H52C)=Sof(H52D)=
 Sof(O53A)=Sof(C54A)=Sof(H54C)=Sof(H54D)=Sof(C55A)=Sof(H55C)=Sof(H55D)=
 Sof(O56A)=Sof(C57A)=Sof(H57C)=Sof(H57D)=Sof(C58A)=Sof(H58C)=Sof(H58D)=
 Sof(C61A)=Sof(H61C)=Sof(H61D)=Sof(C62A)=Sof(H62C)=Sof(H62D)=Sof(O63A)=
 Sof(C64A)=Sof(H64C)=Sof(H64D)=Sof(C65A)=Sof(H65C)=Sof(H65D)=Sof(O66A)=
 Sof(C67A)=Sof(H67C)=Sof(H67D)=Sof(C68A)=Sof(H68C)=Sof(H68D)=1-FVAR(1)
 Sof(N41)=Sof(N42)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=
 Sof(O43)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(O46)=
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C51)=Sof(H51A)=
 Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(O53)=Sof(C54)=Sof(H54A)=Sof(H54B)=
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(O56)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(C58)=
 Sof(H58A)=Sof(H58B)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(C62)=Sof(H62A)=Sof(H62B)=
 Sof(O63)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(O66)=
 Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(C68)=Sof(H68A)=Sof(H68B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 N3(H3), C7(H7), C10(H10), C13(H13), C16(H16), N6(H6), C25(H25), C28(H28),
 C31(H31), C34(H34)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B),
  C24(H24A,H24B), C38(H38A,H38B), C39(H39A,H39B), C41(H41A,H41B), C42(H42A,
 H42B), C44(H44A,H44B), C45(H45A,H45B), C47(H47A,H47B), C48(H48A,H48B),
 C51(H51A,H51B), C52(H52A,H52B), C54(H54A,H54B), C55(H55A,H55B), C57(H57A,H57B),
  C58(H58A,H58B), C61(H61A,H61B), C62(H62A,H62B), C64(H64A,H64B), C65(H65A,
 H65B), C67(H67A,H67B), C68(H68A,H68B), C41A(H41C,H41D), C42A(H42C,H42D),
 C44A(H44C,H44D), C45A(H45C,H45D), C47A(H47C,H47D), C48A(H48C,H48D), C51A(H51C,
 H51D), C52A(H52C,H52D), C54A(H54C,H54D), C55A(H55C,H55D), C57A(H57C,H57D),
 C58A(H58C,H58D), C61A(H61C,H61D), C62A(H62C,H62D), C64A(H64C,H64D), C65A(H65C,
 H65D), C67A(H67C,H67D), C68A(H68C,H68D)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              95278
_shelx_hkl_checksum              55303
_olex2_submission_special_instructions 'No special instructions were received'