Quantified structural speciation in self-sorted CoII6L<sub>4</sub> cage systems.
Rizzuto, Felix J.; Kieffer, Marion; Nitschke, Jonathan R.; Chemical science 9 (2018) 1925–1930; doi:10.1039/c7sc04927g

data_1548651
_publ_section_title
;
 Quantified structural speciation in self-sorted CoII6L<sub>4</sub> cage
 systems.
;
_journal_issue                   7
_journal_name_full               'Chemical science'
_journal_page_first              1925
_journal_page_last               1930
_journal_paper_doi               10.1039/c7sc04927g
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety
'(Co6 C228 H144 N40), 5(B F4), 7(C F3 S O3), 7(C2 H3 N), 0.25(C6 H14 O)'
_chemical_formula_sum            'C250.5 H168.5 B5 Co6 F41 N47 O21.25 S7'
_chemical_formula_weight         5587.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-08-10 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                93.2080(10)
_cell_angle_beta                 101.6240(10)
_cell_angle_gamma                118.5210(10)
_cell_formula_units_Z            2
_cell_length_a                   21.2508(3)
_cell_length_b                   21.6182(2)
_cell_length_c                   39.5929(4)
_cell_measurement_reflns_used    41347
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.3100
_cell_measurement_theta_min      1.5440
_cell_volume                     15407.3(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
GDA 8.44, generic data acquisition software
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris Pilatus 2M'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       '\f rotation with 0.1 degree frames'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Diamond Light Source Beamline I19'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            142112
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        21.311
_diffrn_reflns_theta_max         21.311
_diffrn_reflns_theta_min         1.551
_exptl_absorpt_coefficient_mu    0.409
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.5776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       block
_exptl_crystal_F_000             5677
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.568
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3468
_refine_ls_number_reflns         37722
_refine_ls_number_restraints     8974
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1226
_refine_ls_R_factor_gt           0.1132
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w={1-exp[-20.0000(sin\q/\l)^2^)]}/[\s^2^(Fo^2^)+(0.1000P)^2^+25.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2700
_refine_ls_wR_factor_ref         0.2782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30531
_reflns_number_total             37722
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc04927g2.cif
_cod_data_source_block           sad_a_sq
_cod_depositor_comments
'Adding full bibliography for 1548651--1548652.cif.'
_cod_original_cell_volume        15407.3(3)
_cod_original_formula_sum        'C250.50 H168.50 B5 Co6 F41 N47 O21.25 S7'
_cod_database_code               1548651
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.949
_shelx_estimated_absorpt_t_max   0.984
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              2355
_shelx_fab_checksum              93895