Dibenzoarsacrowns: an experimental and computational study on the coordination behaviors.
Sumida, Akifumi; Kobayashi, Ryosuke; Yumura, Takashi; Imoto, Hiroaki; Naka, Kensuke; Chemical communications (Cambridge, England) 57 (2021) 2013–2016; doi:10.1039/d0cc07191a

data_7127706
_publ_section_title
;
 Dibenzoarsacrowns: an experimental and computational study on the
 coordination behaviors.
;
_journal_issue                   16
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2013
_journal_page_last               2016
_journal_paper_doi               10.1039/d0cc07191a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C28 H33 As F6 K O6 P'
_chemical_formula_sum            'C28 H33 As F6 K O6 P'
_chemical_formula_weight         724.53
_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     iterative
_audit_creation_date             2020-10-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-10-29 deposited with the CCDC.	2020-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                75.414(11)
_cell_angle_beta                 83.884(13)
_cell_angle_gamma                88.235(15)
_cell_formula_units_Z            4
_cell_length_a                   10.898(6)
_cell_length_b                   15.024(8)
_cell_length_c                   19.480(10)
_cell_measurement_reflns_used    8339
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      6.09
_cell_volume                     3069(3)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      93.15
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'XtaLAB mini'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31676
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.565
_diffrn_reflns_theta_min         6.724
_exptl_absorpt_coefficient_mu    1.372
_exptl_absorpt_correction_T_max  0.681
_exptl_absorpt_correction_T_min  0.580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       prism
_exptl_crystal_F_000             1480
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and hexane  by solvent layering'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.185
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         13822
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0453P)^2^+2.1287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0922
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12418
_reflns_number_total             13822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07191a2.cif
_cod_data_source_block           4+KPF6
_cod_depositor_comments
'Adding full bibliography for 7127700--7127710.cif.'
_cod_database_code               7127706
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.700
_shelx_estimated_absorpt_t_min   0.624
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F7A) = Uanis(F7B)
Uanis(F10B) = Uanis(F10A)
Uanis(F8B) = Uanis(F8A)
Uanis(F9A) = Uanis(F9B)
3. Rigid body (RIGU) restrains
 P2, F7B, F11, F9B, F8B, F10B, F12
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F7A, P2, F11, F8A, F10A, F12, F9A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(F8A)=Sof(F7A)=Sof(F10A)=Sof(F9A)=1-FVAR(1)
 Sof(F7B)=Sof(F9B)=Sof(F8B)=Sof(F10B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 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),
  C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,
 H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
 C44(H44A,H44B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C18(H18), C19(H19), C20(H20), C21(H21),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
  C33(H33), C46(H46), C47(H47), C48(H48), C49(H49), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56)
;
_shelx_res_checksum              49885
_shelx_hkl_checksum              98046
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a glass fibre'
_olex2_submission_special_instructions 'No special instructions were received'