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_7130458
_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         'C36 H72 As2'
_chemical_formula_sum            'C36 H72 As2'
_chemical_formula_weight         654.77
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-22
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-06-01 deposited with the CCDC.	2022-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                85.931(2)
_cell_angle_beta                 83.106(2)
_cell_angle_gamma                61.125(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2624(6)
_cell_length_b                   9.3808(6)
_cell_length_c                   25.6699(17)
_cell_measurement_reflns_used    9418
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      65.155
_cell_measurement_theta_min      5.207
_cell_volume                     1938.8(2)
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0347
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26789
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        65.585
_diffrn_reflns_theta_max         65.585
_diffrn_reflns_theta_min         3.469
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.255
_exptl_absorpt_correction_T_max  0.3795
_exptl_absorpt_correction_T_min  0.2800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0766 before and 0.0505 after correction.
The Ratio of minimum to maximum transmission is 0.7378.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.057
_exptl_crystal_size_mid          0.014
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0523P)^2^+0.5141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6004
_reflns_number_total             6586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03235j2.cif
_cod_data_source_block           sz02110a
_cod_database_code               7130458
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.882
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C24(H24A,H24B), C13(H13A,H13B), C6(H6A,H6B), C5(H5A,H5B),
 C12(H12A,H12B), C36(H36A,H36B), C3(H3A,H3B), C17(H17A,H17B), C20(H20A,H20B),
 C14(H14A,H14B), C23(H23A,H23B), C16(H16A,H16B), C19(H19A,H19B), C4(H4A,H4B),
 C11(H11A,H11B), C1(H1A,H1B), C9(H9A,H9B), C22(H22A,H22B), C18(H18A,H18B),
 C21(H21A,H21B), C25(H25A,H25B), C31(H31A,H31B), C8(H8A,H8B), C15(H15A,H15B),
 C28(H28A,H28B), C35(H35A,H35B), C7(H7A,H7B), C33(H33A,H33B), C10(H10A,H10B),
 C34(H34A,H34B), C30(H30A,H30B), C29(H29A,H29B), C27(H27A,H27B), C32(H32A,H32B),
  C26(H26A,H26B)
;
_shelx_res_checksum              34996
_olex2_submission_special_instructions 'No special instructions were received'