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_7127709
_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 Na O6 P'
_chemical_formula_sum            'C28 H33 As F6 Na O6 P'
_chemical_formula_weight         708.42
_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     direct
_audit_creation_date             2020-09-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-09-29 deposited with the CCDC.	2020-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                71.84(3)
_cell_angle_beta                 78.83(4)
_cell_angle_gamma                71.16(3)
_cell_formula_units_Z            4
_cell_length_a                   10.866(9)
_cell_length_b                   14.725(13)
_cell_length_c                   21.75(2)
_cell_measurement_reflns_used    4532
_cell_measurement_temperature    93
_cell_measurement_theta_max      54.971
_cell_measurement_theta_min      6.150
_cell_volume                     3113(5)
_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    'SIR2004  (Burla et al.,  2007)'
_diffrn_ambient_temperature      93
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'XtaLAB mini'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_unetI/netI     0.0994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.953
_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       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30280
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.978
_diffrn_reflns_theta_min         3.035
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.8110
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.756
_refine_diff_density_min         -1.667
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.0048(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         14299
_refine_ls_number_restraints     201
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1434
_refine_ls_R_factor_gt           0.1082
_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^)+(0.0407P)^2^+31.8865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2318
_refine_ls_wR_factor_ref         0.2511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9410
_reflns_number_total             14299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07191a2.cif
_cod_data_source_block           4+NaPF6
_cod_depositor_comments
'Adding full bibliography for 7127700--7127710.cif.'
_cod_original_cell_volume        3112(5)
_cod_database_code               7127709
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.791
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C39-C40 \\sim C39A-C40
 with sigma of 0.02
 C41-C42A \\sim C41A-C42A
 with sigma of 0.02
 C40-C39A \\sim C40A-C39A
 with sigma of 0.02
 C43-C44 \\sim C43A-C44
 with sigma of 0.02
 O10-C41 \\sim O10-C41A
 with sigma of 0.02
 O10-C40 \\sim O10-C40A
 with sigma of 0.02
 O12B-C44 \\sim O12B-C44A
 with sigma of 0.02
 C41-C42 \\sim C41A-C42
 with sigma of 0.02
 C39-C40 \\sim C39-C40A
 with sigma of 0.02
 O11-C43 \\sim O11-C43A
 with sigma of 0.02
 C43-C44A \\sim C43A-C44A
 with sigma of 0.02
 C41-C42 \\sim C41-C42A
 with sigma of 0.02
 C43-C44 \\sim C43-C44A
 with sigma of 0.02
 O11-C42 \\sim O11-C42A
 with sigma of 0.02
 C44-O12A \\sim C44A-O12A
 with sigma of 0.02
 O8-C37 \\sim O8-C37A
 with sigma of 0.02
 C37-C38B \\sim C37A-C38B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C39A \\sim C39: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C40A \\sim C40: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C41A \\sim C41: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C44A \\sim C44: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C38B \\sim C38A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
O9AB \\sim O9AA: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
O9AB: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
O8 \\sim O8A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O11 \\sim O11A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
O10 \\sim O10A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C37 \\sim C37A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C38B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
C37A \\sim C37: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
F11B \\sim F11A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
F8A \\sim F8B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
F7A \\sim F7B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
F12A \\sim F12B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C43A \\sim C43: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(O8) = Uanis(O8A)
Uanis(C45B) = Uanis(C45A)
4. Rigid body (RIGU) restrains
 C36, O8, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C37A, O8A, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C50A, C45A, C46A, C47A, C48A, C49A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C50B, C45B, C46B, C47B, C48B, C49B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O9AB, C38A, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C38B, C37A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C38B, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41, C42A, O11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O8)=Sof(O10)=Sof(O11)=Sof(O12B)=Sof(H36a)=Sof(H36b)=Sof(C37)=Sof(H37a)=
 Sof(H37b)=Sof(C39)=Sof(H39a)=Sof(H39b)=Sof(C40)=Sof(H40a)=Sof(H40b)=Sof(C41)=
 Sof(H41a)=Sof(H41b)=Sof(C44)=Sof(H44a)=Sof(H44b)=Sof(C50B)=Sof(C45B)=Sof(C46B)=
 Sof(H46B)=Sof(C47B)=Sof(H47B)=Sof(C48B)=Sof(H48B)=Sof(C49B)=Sof(H49B)=
 Sof(As2A)=Sof(C43A)=Sof(H43c)=Sof(H43d)=Sof(C42A)=Sof(H42c)=Sof(H42d)=
 Sof(O9AB)=Sof(C38A)=Sof(H38c)=Sof(H38d)=1-FVAR(1)
 Sof(As2B)=Sof(H36c)=Sof(H36d)=Sof(C38B)=Sof(H38a)=Sof(H38b)=Sof(C42)=
 Sof(H42a)=Sof(H42b)=Sof(C43)=Sof(H43a)=Sof(H43b)=Sof(C50A)=Sof(C45A)=Sof(C46A)=
 Sof(H46A)=Sof(C47A)=Sof(H47A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(H49A)=
 Sof(O12A)=Sof(C44A)=Sof(H44c)=Sof(H44d)=Sof(O8A)=Sof(O11A)=Sof(C41A)=Sof(H41c)=
 Sof(H41d)=Sof(O10A)=Sof(C39A)=Sof(H39c)=Sof(H39d)=Sof(C37A)=Sof(H37c)=
 Sof(H37d)=Sof(C40A)=Sof(H40c)=Sof(H40d)=Sof(O9AA)=FVAR(1)
 Sof(F7B)=Sof(F8B)=Sof(F11B)=Sof(F12B)=1-FVAR(2)
 Sof(F7A)=Sof(F11A)=Sof(F12A)=Sof(F8A)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b), C11(H11a,H11b),
 C38(H38e,H38f), C13(H13a,H13b), C14(H14a,H14b), C15(H15a,H15b), C16(H16a,H16b),
  C35(H35a,H35b), C36(H36c,H36d), C36(H36a,H36b), C37(H37a,H37b), C38B(H38a,
 H38b), C39(H39a,H39b), C40(H40a,H40b), C41(H41a,H41b), C42(H42a,H42b),
 C43(H43a,H43b), C44(H44a,H44b), C44A(H44c,H44d), C43A(H43c,H43d), C42A(H42c,
 H42d), C41A(H41c,H41d), C39A(H39c,H39d), C37A(H37c,H37d), C40A(H40c,H40d),
 C38A(H38c,H38d)
6.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), C32(H32), C33(H33),
  C46B(H46B), C47B(H47B), C48B(H48B), C49B(H49B), C52(H52), C53(H53), C54(H54),
 C55(H55), C56(H56), C46A(H46A), C47A(H47A), C48A(H48A), C49A(H49A), C31(H31)
6.c Fitted hexagon refined as free rotating group:
 C50B(C45B,C46B,C47B,C48B,C49B), C50A(C45A,C46A,C47A,C48A,C49A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              55126
_shelx_hkl_checksum              85588
_shelx_fab_checksum              35062
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a glass fibre'
_olex2_submission_special_instructions 'No special instructions were received'