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_7710942
_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         'C20 H48 B2 Cl2 N6 O8 P4 Pt2, 2(C F3 O3 S)'
_chemical_formula_sum            'C22 H48 B2 Cl2 F6 N6 O14 P4 Pt2 S2'
_chemical_formula_weight         1405.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-10-20
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.9286(8)
_cell_length_b                   18.9042(4)
_cell_length_c                   18.5116(4)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.294
_cell_volume                     9073.6(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Nonius Kappa APEX II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            78652
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.155
_exptl_absorpt_coefficient_mu    6.598
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0942 before and 0.0827 after correction.
The Ratio of minimum to maximum transmission is 0.8064.
The \l/2 correction factor is not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.058
_exptl_crystal_description       needle
_exptl_crystal_F_000             5440
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.327
_refine_diff_density_min         -1.605
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details
;
 Flack x determined using 3391 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         7975
_refine_ls_number_restraints     807
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+72.6144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0688
_reflns_Friedel_coverage         0.930
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                7630
_reflns_number_total             7975
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01482c2.cif
_cod_data_source_block           dal2114p2_a
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               7710942
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
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
 S111-O112 \\sim S111-O113 \\sim S111-O114 \\sim S101_$1-O102_$1 \\sim
S101_$1-O103_$1 ~
 S101_$1-O104_$1 \\sim S121_$2-O122_$2 \\sim S121_$2-O123_$2 \\sim
S121_$2-O124_$2
 with sigma of 0.02
 C105-F106 \\sim C105-F107 \\sim C105-F108 \\sim C115_$3-F116_$3 \\sim
C115_$3-F117_$3 ~
 C115_$3-F118_$3 \\sim C125_$4-F126_$4 \\sim C125_$4-F127_$4 \\sim
C125_$4-F128_$4
 with sigma of 0.02
 S101-C105 \\sim S111_$3-C115_$3 \\sim S121_$4-C125_$4
 with sigma of 0.02
 O102-O103 \\sim O102-O104 \\sim O103-O104 \\sim O112_$3-O113_$3 \\sim
O112_$3-O114_$3 ~
 O113_$3-O114_$3 \\sim O122_$4-O123_$4 \\sim O122_$4-O124_$4 \\sim
O123_$4-O124_$4
 with sigma of 0.02
 F106-F107 \\sim F106-F108 \\sim F107-F108 \\sim F116_$3-F117_$3 \\sim
F116_$3-F118_$3 ~
 F117_$3-F118_$3 \\sim F126_$4-F127_$4 \\sim F126_$4-F128_$4 \\sim
F127_$4-F128_$4
 with sigma of 0.02
 S101-F106 \\sim S101-F107 \\sim S101-F108 \\sim S111_$3-F116_$3 \\sim
S111_$3-F117_$3 ~
 S111_$3-F118_$3 \\sim S121_$4-F126_$4 \\sim S121_$4-F127_$4 \\sim
S121_$4-F128_$4
 with sigma of 0.02
 C105-O102 \\sim C105-O103 \\sim C105-O104 \\sim C115_$3-O112_$3 \\sim
C115_$3-O113_$3 ~
 C115_$3-O114_$3 \\sim C125_$4-O122_$4 \\sim C125_$4-O123_$4 \\sim
C125_$4-O124_$4
 with sigma of 0.02
 N1-C1 \\sim N1-C1'
 with sigma of 0.02
 C4-C3 \\sim C4-C3'
 with sigma of 0.02
 N3-C3 \\sim N3-C3'
 with sigma of 0.02
 C2-C3 \\sim C2'-C3'
 with sigma of 0.02
 C4-C5 \\sim C4-C5'
 with sigma of 0.02
 N2-C6 \\sim N2-C6'
 with sigma of 0.02
 C1-C2 \\sim C1'-C2'
 with sigma of 0.02
 C5-C6 \\sim C5'-C6'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S111 \\sim O112 \\sim O113 \\sim O114 \\sim C115 \\sim F116 \\sim F117 \\sim
F118 \\sim S11' \\sim O12' \\sim O13' \\sim O14' \\sim C15' \\sim F16' \\sim
F17' \\sim F18' \\sim S121 \\sim O122 \\sim O123 \\sim O124 \\sim C125 \\sim
F126 \\sim F127 \\sim F128: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C3) = Uanis(C3')
Uanis(S111) = Uanis(S11')
Uanis(C1) = Uanis(C1')
Uanis(C2) = Uanis(C2')
Uanis(C5) = Uanis(C5')
Uanis(C6) = Uanis(C6')
4. Rigid body (RIGU) restrains
 S111, O112, O113, O114, C115, F116, F117, F118, S11', O12', O13', O14', C15',
 F16', F17', F18', S121, O122, O123, O124, C125, F126, F127, F128
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{S111, O112, O113, O114, C115, F116, F117, F118} sigma for 1-2: 0.005, 1-3:
0.005
as
{S11', O12', O13', O14', C15', F16', F17', F18'}
6. Others
 Sof(C1')=Sof(H1'A)=Sof(H1'B)=Sof(C2')=Sof(H2'A)=Sof(H2'B)=Sof(C3')=Sof(H3'A)=
 Sof(H3'B)=Sof(H4BC)=Sof(H4BD)=Sof(C5')=Sof(H5'A)=Sof(H5'B)=Sof(C6')=Sof(H6'A)=
 Sof(H6'B)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(H4AA)=Sof(H4AB)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(1)
 Fixed Sof: S111(0.25) O112(0.25) O113(0.25) O114(0.25) C115(0.25) F116(0.25)
 F117(0.25) F118(0.25) S11'(0.25) O12'(0.25) O13'(0.25) O14'(0.25) C15'(0.25)
 F16'(0.25) F17'(0.25) F18'(0.25) S121(0.5) O122(0.5) O123(0.5) O124(0.5)
 C125(0.5) F126(0.5) F127(0.5) F128(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1'(H1'A,H1'B), C2(H2A,H2B), C2'(H2'A,H2'B), C3(H3A,H3B),
 C3'(H3'A,H3'B), C4(H4AA,H4AB), C4(H4BC,H4BD), C5(H5A,H5B), C5'(H5'A,H5'B),
 C6(H6A,H6B), C6'(H6'A,H6'B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
7.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C)
;
_shelx_res_checksum              19522
_shelx_hkl_checksum              53645
_olex2_submission_special_instructions 'No special instructions were received'