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_7130459
_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 O2, 4(H2 O)'
_chemical_formula_sum            'C42 H92 As2 O6'
_chemical_formula_weight         842.99
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-06-01 deposited with the CCDC.	2022-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                72.297(2)
_cell_angle_beta                 84.548(2)
_cell_angle_gamma                88.073(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6319(6)
_cell_length_b                   13.4245(10)
_cell_length_c                   20.7781(15)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      65.325
_cell_measurement_theta_min      4.486
_cell_volume                     2283.3(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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30552
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        65.565
_diffrn_reflns_theta_max         65.565
_diffrn_reflns_theta_min         3.456
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.123
_exptl_absorpt_correction_T_max  0.4649
_exptl_absorpt_correction_T_min  0.3677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1167 before and 0.0757 after correction.
The Ratio of minimum to maximum transmission is 0.7909.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.085
_refine_diff_density_max         1.141
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         7756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0678
_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^)+(0.0133P)^2^+17.5123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1707
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7296
_reflns_number_total             7756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03235j2.cif
_cod_data_source_block           sz02136
_cod_database_code               7130459
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.725
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9765(7)
 0.0235(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3.a Riding coordinates:
 O1W(H3WA,H1WA), O3W(H1WB,H3WB)
3.b Free rotating group:
 O2W(H2WA,H2WB), O4W(H4WA,H4WB)
3.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
  C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
 C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B)
;
_shelx_res_checksum              11713
_olex2_submission_special_instructions 'No special instructions were received'