Post-assembly Modification of Phosphine Cages Controls Host-Guest Behavior.
McTernan, Charlie T.; Ronson, Tanya K.; Nitschke, Jonathan R.; Journal of the American Chemical Society 141 (2019) 6837–6842; doi:10.1021/jacs.9b02604

data_4128117
_publ_section_title
;
 Post-assembly Modification of Phosphine Cages Controls Host-Guest
 Behavior.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6837
_journal_page_last               6842
_journal_paper_doi               10.1021/jacs.9b02604
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety
;    
'C160 H120 N48 P4 Zn4, 0.75(C2 F6 N O4 S2), 2.5(C6 H6), 1.25(I4 Zn),
    0.75(I3 Zn O H2), 0.5(C2 H3 N), 0.75(H2 O), 1.75(I), [+ 6.25 anions]'
;
_chemical_formula_sum
'C177.5 H139.5 F4.5 I9 N49.25 O4.5 P4 S1.5 Zn6'
_chemical_formula_weight         4826.17
_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   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90.804(2)
_cell_angle_beta                 102.438(2)
_cell_angle_gamma                104.311(2)
_cell_formula_units_Z            2
_cell_length_a                   21.1660(4)
_cell_length_b                   21.8072(4)
_cell_length_c                   35.8636(7)
_cell_measurement_reflns_used    15064
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.8098459159
_cell_measurement_theta_min      0.559650875387
_cell_volume                     15623.8(6)
_computing_cell_refinement
;
DIALS 2theta refinement, DIALS 1.7.1-g93fc14f4-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 1.7.1-g93fc14f4-release
pointless (Evans, P., 2006)
XIA2 0.5.432-ga4ad5612-dials-1.7 (Winter, G., 2010)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon counting pixel array'
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_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  0.0511
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            40437
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        18.248
_diffrn_reflns_theta_max         18.248
_diffrn_reflns_theta_min         0.565
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.291
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.97067650853
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.052: AIMLESS, version 0.6.2 : 15/01/18
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.026
_exptl_crystal_description       block
_exptl_crystal_F_000             4734
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2523
_refine_ls_number_reflns         23203
_refine_ls_number_restraints     4626
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.1500
_refine_ls_R_factor_gt           0.1265
_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^+75.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3510
_refine_ls_wR_factor_ref         0.3638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14475
_reflns_number_total             23203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02604_si_002.cif
_cod_data_source_block           ctm179zn_sq
_cod_original_cell_volume        15623.8(5)
_cod_original_formula_sum
'C177.50 H139.50 F4.50 I9 N49.25 O4.50 P4 S1.50 Zn6'
_cod_database_code               4128117
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.962
_shelx_res_checksum              21219
_shelx_hkl_checksum              53443
_shelx_fab_checksum              45938