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_7710941
_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         '0.5(C20 H52 B2 Cl4 N6 O10 P4 Pt2)'
_chemical_formula_sum            'C10 H26 B Cl2 N3 O5 P2 Pt'
_chemical_formula_weight         607.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-01
_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                 94.505(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0870(11)
_cell_length_b                   14.6292(12)
_cell_length_c                   16.036(3)
_cell_measurement_reflns_used    1245
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.66
_cell_measurement_theta_min      2.53
_cell_volume                     1891.3(5)
_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_temperature      100.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Nonius Kappa APEX II'
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32167
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.526
_exptl_absorpt_coefficient_mu    7.896
_exptl_absorpt_correction_T_max  0.8682
_exptl_absorpt_correction_T_min  0.6132
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0729 before and 0.0563 after correction.
The Ratio of minimum to maximum transmission is 0.7063.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.132
_exptl_crystal_description       plate
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.065
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.092
_refine_diff_density_min         -1.904
_refine_diff_density_rms         0.196
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.290
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         6500
_refine_ls_number_restraints     1257
_refine_ls_restrained_S_all      1.413
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+23.9761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_full    0.955
_reflns_Friedel_fraction_max     0.955
_reflns_number_gt                6129
_reflns_number_total             6500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01482c2.cif
_cod_data_source_block           dal1941z4_c
_cod_original_cell_volume        1891.3(4)
_cod_database_code               7710941
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.858
_shelx_estimated_absorpt_t_min   0.628
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(3)
 0.50(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 Pt1-P1 \\sim Pt1-P1A \\sim Pt1-P2 \\sim Pt1-P2A \\sim Pt2-P4 \\sim Pt2-P4A
\\sim Pt2-P3 \\sim Pt2-P3A
 with sigma of 0.01
 P1-O11 \\sim P1A-O11A \\sim P1-O12 \\sim P1A-O12A \\sim P2-O21 \\sim P2A-O21A
\\sim P2-O22 \\sim P2A-O22A
 \\sim P3-O31 \\sim P3-O32 \\sim P3A-O31A \\sim P3A-O32A \\sim P4-O41 \\sim
P4-O42 \\sim P4A-O41A \\sim P4A-O42A
 with sigma of 0.01
 O11-C11 \\sim O11A-C11A \\sim O12-C12 \\sim O12A-C12A \\sim O21-C21 \\sim
O21A-C21A \\sim O22-C22 ~
 O22A-C22A \\sim O31-C31 \\sim O32-C32 \\sim O31A-C31A \\sim O32A-C32A \\sim
O41-C41 \\sim O42-C42 ~
 O41A-C41A \\sim O42A-C42A
 with sigma of 0.01
 B1-O1 \\sim B2-O2
 with sigma of 0.01
 B1-N3 \\sim B2-N6
 with sigma of 0.01
 B1-N1 \\sim B1-N2 \\sim B2-N4 \\sim B2-N5
 with sigma of 0.01
 P1-N1 \\sim P1A-N1 \\sim P2-N2 \\sim P2A-N2 \\sim P3-N5 \\sim P3A-N5 \\sim
P4-N4 \\sim P4A-N4
 with sigma of 0.01
 O11-O12 \\sim O11A-O12A \\sim O21-O22 \\sim O21A-O22A \\sim O31-O32 \\sim
O31A-O32A \\sim O41-O42 ~
 O41A-O42A
 with sigma of 0.01
 P1-C11 \\sim P1-C12 \\sim P1A-C11A \\sim P1A-C12A \\sim P2-C21 \\sim P2-C22
\\sim P2A-C21A \\sim P2A-C22A
 \\sim P3-C31 \\sim P3-C32 \\sim P3A-C31A \\sim P3A-C32A \\sim P4-C41 \\sim
P4-C42 \\sim P4A-C41A \\sim P4A-C42A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C11) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(P1) \\sim Ueq, Uanis(O12)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(O11A) \\sim Ueq,
Uanis(P1A) \\sim Ueq, Uanis(O12A) \\sim Ueq, Uanis(C12A) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C21) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(P2) \\sim Ueq, Uanis(O22)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(O21A) \\sim Ueq,
Uanis(P2A) \\sim Ueq, Uanis(O22A) \\sim Ueq, Uanis(C22A) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C41) \\sim Ueq, Uanis(O41) \\sim Ueq, Uanis(P4) \\sim Ueq, Uanis(O42)
\\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C41A) \\sim Ueq, Uanis(O41A) \\sim Ueq,
Uanis(P4A) \\sim Ueq, Uanis(O42A) \\sim Ueq, Uanis(C42A) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C31) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(P3) \\sim Ueq, Uanis(O32)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(O31A) \\sim Ueq,
Uanis(P3A) \\sim Ueq, Uanis(O32A) \\sim Ueq, Uanis(C32A) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Sof(P1A)=Sof(O11A)=Sof(O12A)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=
 Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(P1)=Sof(O11)=Sof(O12)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=
 Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Sof(P4)=Sof(O41)=Sof(O42)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=
 Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(P2A)=Sof(O21A)=Sof(O22A)=Sof(C21A)=Sof(H21D)=
 Sof(H21E)=Sof(H21F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(2)
 Sof(P2)=Sof(O21)=Sof(O22)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=
 Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(P4A)=Sof(O41A)=Sof(O42A)=Sof(C41A)=Sof(H41D)=
 Sof(H41E)=Sof(H41F)=Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=FVAR(2)
 Sof(P3A)=Sof(O31A)=Sof(O32A)=Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=
 Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(3)
 Sof(P3)=Sof(O31)=Sof(O32)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=
 Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(3)
7.a Ternary CH refined with riding coordinates:
 N3(H3), N6(H6)
7.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),
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C28(H28A,H28B),
  C29(H29A,H29B)
7.c Me refined with riding coordinates:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C32(H32A,H32B,H32C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C11A(H11D,H11E,H11F), C12A(H12D,H12E,H12F), C21A(H21D,H21E,H21F), C22A(H22D,
 H22E,H22F), C31A(H31D,H31E,H31F), C32A(H32D,H32E,H32F), C41A(H41D,H41E,H41F),
 C42A(H42D,H42E,H42F)
7.d Tetrahedral OH refined with riding coordinates:
 O1(H1), O2(H2)
7.e Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C)
;
_shelx_res_checksum              6753
_shelx_hkl_checksum              188
_olex2_submission_special_instructions 'No special instructions were received'