Incarceration of one or two phosphate or arsenate species within nanojars, capped nanojars and nanohelicages: helical chirality from two closely-spaced, head-to-head PO4^3-^ or AsO4^3-^ ions
Gellert Mezei; Chem.Commun. 51 (2015) 10341–; doi:10.1039/C5cc03005F

data_7117306
_publ_section_title
;
 Incarceration of one or two phosphate or arsenate species within
 nanojars, capped nanojars and nanohelicages: helical chirality from two
 closely-spaced, head-to-head PO4^3-^ or AsO4^3-^ ions
;
_journal_name_full               Chem.Commun.
_journal_page_first              10341
_journal_paper_doi               10.1039/C5cc03005F
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C104 H149 Br1.5 Cu15 N39.5 O19 P2'
_chemical_formula_weight         3391.52
_chemical_properties_physical    Efflorescent
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-04-07 deposited with the CCDC.
2015-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.2540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1774(2)
_cell_length_b                   24.4000(3)
_cell_length_c                   33.5490(4)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.71
_cell_measurement_theta_min      2.24
_cell_volume                     13686.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1314
_diffrn_reflns_av_unetI/netI     0.0793
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            197389
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.083
_diffrn_reflns_theta_min         1.042
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.811
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6074
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       block
_exptl_crystal_F_000             6876
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: nitrobenzene, bromobenzene, hexanes'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.266
_refine_diff_density_min         -2.340
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1593
_refine_ls_number_reflns         24276
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.0688
_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^)+(0.0606P)^2^+272.0120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1617
_refine_ls_wR_factor_ref         0.1895
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                15747
_reflns_number_total             24276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc03005f2.cif
_cod_data_source_block           4
_cod_original_formula_sum        'C104 H149 Br1.50 Cu15 N39.50 O19 P2'
_cod_database_code               7117306
_shelxl_version_number           2014/6
_shelx_res_checksum              47990