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_4128119
_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 Ni4, 2.25(C2 F6 N O4 S2), 9.75(C6 H6), 1.1(I4 Ni),
   2.75(C2 H3 N), 4.1(I), [+ 3.45 anions]'
;
_chemical_formula_sum
'C228.5 H186.75 F13.5 I8.5 N53 Ni5.1 O9 P4 S4.5'
_chemical_formula_weight         5721.77
_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                89.9610(10)
_cell_angle_beta                 84.2150(10)
_cell_angle_gamma                65.8950(10)
_cell_formula_units_Z            2
_cell_length_a                   21.1855(2)
_cell_length_b                   24.1723(2)
_cell_length_c                   33.8253(3)
_cell_measurement_reflns_used    51451
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.4331340098
_cell_measurement_theta_min      0.584060727671
_cell_volume                     15715.3(3)
_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 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0479
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            148944
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        24.208
_diffrn_reflns_theta_max         24.208
_diffrn_reflns_theta_min         0.587
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.97710440761
_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            'green brown'
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       block
_exptl_crystal_F_000             5695
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.573
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3084
_refine_ls_number_reflns         53682
_refine_ls_number_restraints     5754
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0901
_refine_ls_shift/su_max          0.005
_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^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2854
_refine_ls_wR_factor_ref         0.3003
_reflns_Friedel_coverage         0.000
_reflns_number_gt                35894
_reflns_number_total             53682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02604_si_004.cif
_cod_data_source_block           ctm179ni_sq
_cod_original_formula_sum
'C228.50 H186.75 F13.50 I8.50 N53 Ni5.10 O9 P4 S4.50'
_cod_database_code               4128119
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.978
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              6703
_shelx_hkl_checksum              20197
_shelx_fab_checksum              4095