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_1548652
_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 C252 H180 N60), 5.5(C B11 H12), 6.5(C F3 S O3), (C4 H10 O), 2.5(C2 H3 N)'
_chemical_formula_sum
'C273 H263.5 B60.5 Co6 F19.5 N62.5 O20.5 S6.5'
_chemical_formula_weight         6334.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                68.1130(17)
_cell_angle_beta                 88.8092(17)
_cell_angle_gamma                66.5154(14)
_cell_formula_units_Z            2
_cell_length_a                   25.0303(4)
_cell_length_b                   26.7592(5)
_cell_length_c                   34.5514(7)
_cell_measurement_reflns_used    8017
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.9388
_cell_measurement_theta_min      1.6107
_cell_volume                     19472.1(7)
_computing_cell_refinement       'XIA2 0.4.0.331-g9691117'
_computing_data_collection       'GDA 8.44; generic data acquisition software'
_computing_data_reduction        'XIA2 0.4.0.331-g9691117'
_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 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0412
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38843
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        16.681
_diffrn_reflns_theta_max         16.681
_diffrn_reflns_theta_min         0.939
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_T_max  1.0108
_exptl_absorpt_correction_T_min  0.9934
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.018: AIMLESS, version 0.5.27 : 18/05/16
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics

Run via XIA2 0.5.53-gee81713-dials-1.3-patch135dmin, DIALS 1.3.4-g9f5e5cd-release, DIALS/i19 0.91-g03fbaed
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_description       prism
_exptl_crystal_F_000             6494
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.055
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4178
_refine_ls_number_reflns         22663
_refine_ls_number_restraints     12498
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.1399
_refine_ls_R_factor_gt           0.1179
_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^+30.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3293
_refine_ls_wR_factor_ref         0.3464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15201
_reflns_number_total             22663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc04927g2.cif
_cod_data_source_block           SHELX_A_SQ
_cod_depositor_comments
'Adding full bibliography for 1548651--1548652.cif.'
_cod_original_cell_volume        19472.2(7)
_cod_original_formula_sum
'C273 H263.50 B60.50 Co6 F19.50 N62.50 O20.50 S6.50'
_cod_database_code               1548652
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.987
_shelx_estimated_absorpt_t_max   0.997
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              18529
_shelx_fab_checksum              60169