Enantiopure [Cs<sup>+</sup>/Xe⊂Cryptophane]⊂Fe<sup>II</sup><sub>4</sub>L<sub>4</sub> Hierarchical Superstructures.
Zhang, Dawei; Ronson, Tanya K.; Greenfield, Jake L.; Brotin, Thierry; Berthault, Patrick; Léonce, Estelle; Zhu, Jun-Long; Xu, Lin; Nitschke, Jonathan R.; Journal of the American Chemical Society 141 (2019) 8339–8345; doi:10.1021/jacs.9b02866

data_4127249
_publ_section_title
;
 Enantiopure
 [Cs<sup>+</sup>/Xe&#x2282;Cryptophane]&#x2282;Fe<sup>II</sup><sub>4</sub>L<sub>4</sub>
 Hierarchical Superstructures.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8339
_journal_page_last               8345
_journal_paper_doi               10.1021/jacs.9b02866
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety
;
'C264 H204 Fe4 N36, C45 H36 O6, 0.36(Cs) 0.45(C2 F6 N1 O4 S2), 
3.175(C H12 B11), 1.125(C2 H3 N), 0.5(C4 H8 O2)'
;
_chemical_formula_sum
'C317.33 H285.48 B34.92 Cs0.36 F2.7 Fe4 N37.58 O8.8 S0.9'
_chemical_formula_weight         5495.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 92.1540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.1172(2)
_cell_length_b                   59.4899(3)
_cell_length_c                   49.3791(6)
_cell_measurement_reflns_used    24173
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.766915075
_cell_measurement_theta_min      0.718528219703
_cell_volume                     91344.0(13)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.12.1-g84e9f68aa-release'
_computing_data_collection       'Diamond GDA'
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.12.1-g84e9f68aa-release (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 0.5.757-g89e4ddb2-dials-1.12 (Winter, G., 2010)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_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       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Diamond Light Source Beamline I19-1'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0971
_diffrn_reflns_av_unetI/netI     0.1271
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            210491
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        17.429
_diffrn_reflns_theta_max         17.429
_diffrn_reflns_theta_min         0.664
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.977369995045
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.065: AIMLESS, version 0.7.3 : 15/08/18
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.799
_exptl_crystal_description       block
_exptl_crystal_F_000             22880
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7212
_refine_ls_number_reflns         62555
_refine_ls_number_restraints     23602
_refine_ls_restrained_S_all      5.683
_refine_ls_R_factor_all          0.1864
_refine_ls_R_factor_gt           0.1183
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3178
_refine_ls_wR_factor_ref         0.3703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27826
_reflns_number_total             62555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02866_si_002.cif
_cod_data_source_block           dzcry
_cod_depositor_comments          'Adding full bibliography for 4127249.cif.'
_cod_original_formula_sum
'C317.33 H285.48 B34.92 Cs0.36 F2.70 Fe4 N37.58 O8.80 S0.90'
_cod_database_code               4127249
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.996
_shelx_estimated_absorpt_t_max   0.998
_shelx_res_checksum              73969
_shelx_hkl_checksum              79372
_shelx_fab_checksum              22499