A surprise landing on the <i>terra incognita</i> of macrocyclic dibridgehead diorganoarsines: syntheses, structures, and reactivities.
Zarcone, Samuel R.; Verardi, Peter J.; Bhuvanesh, Nattamai; Gladysz, John A.; Chemical communications (Cambridge, England) 58 (2022) 8694–8697; doi:10.1039/d2cc03235j

data_7130460
_publ_section_title
;
 A surprise landing on the <i>terra incognita</i> of macrocyclic
 dibridgehead diorganoarsines: syntheses, structures, and reactivities.
;
_journal_issue                   62
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8694
_journal_page_last               8697
_journal_paper_doi               10.1039/d2cc03235j
_journal_volume                  58
_journal_year                    2022
_chemical_formula_moiety         'C42 H84 As2 Cl2 Pt'
_chemical_formula_sum            'C42 H84 As2 Cl2 Pt'
_chemical_formula_weight         1004.92
_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     'SHELXT  (Sheldrick, 2015)'
_audit_creation_date             2021-11-22
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6427)
;
_audit_update_record
;
2022-06-01 deposited with the CCDC.	2022-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.2943(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3117(5)
_cell_length_b                   13.9045(5)
_cell_length_c                   20.1180(6)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      71.710
_cell_measurement_theta_min      3.450
_cell_volume                     4561.7(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Venture (PHOTON III)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59120
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.989
_diffrn_reflns_theta_min         3.527
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.619
_exptl_absorpt_correction_T_max  0.3520
_exptl_absorpt_correction_T_min  0.1685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1097 before and 0.0650 after correction.
The Ratio of minimum to maximum transmission is 0.4787.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethyl ether/methanol'
_exptl_crystal_size_max          0.042
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.618
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         8637
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0349P)^2^+3.8123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0688
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8077
_reflns_number_total             8637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03235j2.cif
_cod_data_source_block           sz0295b
_cod_database_code               7130460
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.782
_shelx_estimated_absorpt_t_min   0.714
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C33A-C32A \\sim C33-C32
 with sigma of 0.02
 C32-C31 \\sim C32A-C31 \\sim C34-C33A \\sim C34-C33
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C31 \\sim C34 \\sim C33 \\sim C32 \\sim C33A \\sim C32A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 C31, C34, C33, C32, C33A, C32A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
5. Others
 Sof(H31C)=Sof(H31D)=Sof(H34C)=Sof(H34D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=
 Sof(C32A)=Sof(H32C)=Sof(H32D)=1-FVAR(1)
 Sof(H31A)=Sof(H31B)=Sof(H34A)=Sof(H34B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C32)=
 Sof(H32A)=Sof(H32B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C16(H16A,H16B), C1(H1A,H1B), C15(H15A,H15B),
 C40(H40A,H40B), C2(H2A,H2B), C42(H42A,H42B), C5(H5A,H5B), C14(H14A,H14B),
 C4(H4A,H4B), C3(H3A,H3B), C27(H27A,H27B), C9(H9A,H9B), C39(H39A,H39B),
 C41(H41A,H41B), C6(H6A,H6B), C13(H13A,H13B), C17(H17A,H17B), C21(H21A,H21B),
 C36(H36A,H36B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C26(H26A,H26B),
  C25(H25A,H25B), C30(H30A,H30B), C19(H19A,H19B), C20(H20A,H20B), C24(H24A,
 H24B), C8(H8A,H8B), C22(H22A,H22B), C35(H35A,H35B), C7(H7A,H7B), C18(H18A,
 H18B), C38(H38A,H38B), C37(H37A,H37B), C23(H23A,H23B), C31(H31A,H31B),
 C31(H31C,H31D), C34(H34A,H34B), C34(H34C,H34D), C33(H33A,H33B), C32(H32A,H32B),
  C33A(H33C,H33D), C32A(H32C,H32D)
;
_shelx_res_checksum              55387
_olex2_submission_special_instructions 'No special instructions were received'