Substituent-controlled racemization of dissymmetric coordination capsules.
Harada, Kentaro; Sekiya, Ryo; Maehara, Takeshi; Haino, Takeharu; Organic & biomolecular chemistry 17 (2019) 4729–4735; doi:10.1039/c9ob00388f

data_7156759
_publ_section_title
;
 Substituent-controlled racemization of dissymmetric coordination
 capsules.
;
_journal_issue                   19
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              4729
_journal_page_last               4735
_journal_paper_doi               10.1039/c9ob00388f
_journal_volume                  17
_journal_year                    2019
_chemical_formula_moiety         '2(C34 H28 N4 O2 Cu), B F4 '
_chemical_formula_sum            'C68 H56 B Cu2 F4 N8 O4'
_chemical_formula_weight         1263.09
_chemical_properties_physical    Oxygen-sensitive
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-02-17T12:23:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-02-17 deposited with the CCDC.    2019-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                74.499(10)
_cell_angle_beta                 79.884(10)
_cell_angle_gamma                87.811(10)
_cell_formula_units_Z            2
_cell_length_a                   10.868(10)
_cell_length_b                   15.852(15)
_cell_length_c                   21.43(2)
_cell_measurement_reflns_used    3025
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      20.95
_cell_measurement_theta_min      2.26
_cell_volume                     3502(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.578
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bluker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotary anticathode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.053
_diffrn_reflns_av_unetI/netI     0.1047
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10235
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         21.042
_diffrn_reflns_theta_min         1.867
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.20
_exptl_crystal_description       block
_exptl_crystal_F_000             1302
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromathane'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.367
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.325
_refine_ls_extinction_coef       0.162(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.873
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         7314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.873
_refine_ls_R_factor_all          0.2041
_refine_ls_R_factor_gt           0.1819
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.2000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4678
_refine_ls_wR_factor_ref         0.4807
_reflns_Friedel_coverage         0
_reflns_number_gt                5370
_reflns_number_total             7314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ob00388f2.cif
_cod_data_source_block           model_complex
_cod_depositor_comments          'Adding full bibliography for 7156759.cif.'
_cod_original_formula_sum        'C68 H56 N8 O4 Cu2 B F4'
_cod_database_code               7156759
_shelxl_version_number           2013-2
_shelx_res_checksum              42044