As-stereogenic C2-symmetric organoarsines: synthesis and enantioselective self-assembly into a dinuclear triple-stranded helicate with copper iodide.
Adachi, Hiroki; Imoto, Hiroaki; Watase, Seiji; Matsukawa, Kimihiro; Naka, Kensuke; Dalton transactions (Cambridge, England : 2003) 44 (2015) 15372–15376; doi:10.1039/c5dt01490e

data_7035359
_publ_section_title
;
 As-stereogenic C2-symmetric organoarsines: synthesis and enantioselective
 self-assembly into a dinuclear triple-stranded helicate with copper
 iodide.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15372
_journal_page_last               15376
_journal_paper_doi               10.1039/c5dt01490e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C54 H48 As6 Br6 Cu2 I2,3.5(C2 H3 N)'
_chemical_formula_sum            'C61 H58.5 As6 Br6 Cu2 I2 N3.5'
_chemical_formula_weight         2150.47
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-05-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-06-03 deposited with the CCDC.
2015-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.0767(3)
_cell_length_b                   18.0767(3)
_cell_length_c                   38.3573(8)
_cell_measurement_reflns_used    25140
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      3.19
_cell_volume                     10854.7(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            5509
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.443
_diffrn_reflns_theta_min         3.187
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.515
_exptl_absorpt_correction_T_max  0.324
_exptl_absorpt_correction_T_min  0.216
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.974
_exptl_crystal_description       block
_exptl_crystal_F_000             6126
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_platon_squeeze_details
; MeCN molecules are randomly disordered in a toroidal void around 
a 3-fold axis
;
_refine_diff_density_max         1.211
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         5509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0510P)^2^+17.6740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4297
_reflns_number_total             5509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01490e2.cif
_cod_data_source_block           CuI-2b
_cod_depositor_comments
'Adding full bibliography for 7035355--7035359.cif.'
_cod_original_cell_volume        10854.6(5)
_cod_original_formula_sum        'C61 H58.50 As6 Br6 Cu2 I2 N3.50'
_cod_database_code               7035359
_shelx_estimated_absorpt_t_max   0.399
_shelx_estimated_absorpt_t_min   0.399
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H) groups
2. Others
 Fixed Sof: C20(0.33333) N4(0.33333)
3.a Me refined with riding coordinates:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14), C15(H15),
 C17(H17), C18(H18)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'