Self-assembly of M4L4 Tetrahedral Cages Incorporating Pendant P=S and P=Se Functionalised Ligands
Butler, Patrick; Kruger, Paul; Ward, Jas S.; Chemical Communications  (2019) –; doi:10.1039/C9CC05443J

data_7123953
_publ_section_title
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 Self-assembly of M4L4 Tetrahedral Cages Incorporating Pendant P=S and
 P=Se Functionalised Ligands
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05443J
_journal_year                    2019
_chemical_formula_moiety         'C144 H108 Co4 N24 O12 P4 Se4, 8(B F4)'
_chemical_formula_sum            'C144 H108 B8 Co4 F32 N24 O12 P4 Se4'
_chemical_formula_weight         3736.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-09-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-03 deposited with the CCDC.    2019-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.41(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   41.505(8)
_cell_length_b                   12.145(2)
_cell_length_c                   41.753(8)
_cell_measurement_reflns_used    2474
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.3
_cell_measurement_theta_min      0.4
_cell_volume                     18684(8)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.399
_diffrn_measured_fraction_theta_max 0.728
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX1 Beamline Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_Laue_measured_fraction_full 0.399
_diffrn_reflns_Laue_measured_fraction_max 0.728
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            21615
_diffrn_reflns_point_group_measured_fraction_full 0.399
_diffrn_reflns_point_group_measured_fraction_max 0.728
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         20.429
_diffrn_reflns_theta_min         1.099
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.250
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       block
_exptl_crystal_F_000             7472
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         6739
_refine_ls_number_restraints     970
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.0947
_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^)+(0.1325P)^2^+385.0347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2495
_refine_ls_wR_factor_ref         0.2724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4599
_reflns_number_total             6739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05443j2.cif
_cod_data_source_block           '[2d]'
_cod_original_cell_volume        18683(8)
_cod_database_code               7123953
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.885
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 F21, B2, F22, F23, F24
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 B4, F41, F42, F43, F44
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 F14, B1, F11, F12, F13
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 F53, B5, F51, F52, F54
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
F21 \\sim B2 \\sim F22 \\sim F23 \\sim F24: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
F42 \\sim B4 \\sim F41 \\sim F43 \\sim F44: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
F14 \\sim B1 \\sim F11 \\sim F12 \\sim F13: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
F53 \\sim B5 \\sim F51 \\sim F52 \\sim F54: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C159, Se1, P1, O11, O12, O13, C111, C131, C151, C116, C112, C136, C132, C156,
 C152, H116, C115, H112, C113, H136, C135, H132, C133, H156, C155, H152, C153,
 C114, H115, H113, C134, H135, H133, C154, H155, H153, N117, N137, N157, Co1,
 C118, Co2, C138, Co2, C158, N217, N257, N124, N224, N264, H118, C119, N157,
 N237, N144, N164, N244, H138, C139, N137, N237, N144, N164, N244, H158, C159,
 C214, C218, C254, C258, C123, C223, C219, C263, C259, C120, C154, C158, C234,
 C238, C143, C163, C243, C239, C140, C134, C138, C234, C238, C143, C139, C163,
 C243, C239, C160, C215, C213, H218, C255, C253, H258, H123, C122, H223, C222,
 C220, H263, C262, C260, H120, C121, C153, C155, H158, C235, C233, H238, C142,
 H143, H163, C162, C160, H243, C242, C240, H140, C141, C133, C135, H138, C235,
 C233, H238, C142, H143, C140, H163, C162, H243, C242, C240, C161, H160, H215,
 C216, C212, H213, H255, C256, C252, H253, H122, H222, C221, H220, H262, C261,
 H260, H121, C152, H153, C156, H155, H235, C236, C232, H233, H142, H162, C161,
 H160, C241, H242, H240, H141, C132, H133, C136, H135, H235, C236, C232, H233,
 H142, C141, H140, H162, C241, H242, H240, H161, H216, C211, H212, H256, C251,
 H252, H221, H261, C151, H152, H156, H236, C231, H232, H161, H241, C131, H132,
 H136, H236, C231, H232, H141, H241, O21, O23, O13, O22, O12, O22, P2, P2, P1,
 Se2, O23, Se2, O21, Se1, O11, C251, C211, C111, C256, C252, C216, C212, C116,
 C112, C255, H256, H252, C253, C215, H216, H212, C213, H116, C115, H112, C113,
 H255, C254, H253, H215, C214, H213, C114, H115, H113, N257, N217, N117, Co1,
 C258, C218, C118, N124, N224, N264, H258, C259, H218, C219, H118, C119, C123,
 C223, C263, C260, C220, C120, H123, C122, H223, C222, H263, C262, C261, H260,
 C221, H220, H120, C121, H122, H222, H262, H261, H221, H121
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
5.a Free rotating group:
 B1(F11,F12,F13,F14), B2(F21,F22,F23,F24), B4(F41,F42,F43,F44), B5(F51,F52,F53,
 F54)
5.b Aromatic/amide H refined with riding coordinates:
 C116(H116), C112(H112), C113(H113), C115(H115), C118(H118), C123(H123),
 C120(H120), C121(H121), C122(H122), C136(H136), C132(H132), C133(H133),
 C135(H135), C138(H138), C142(H142), C143(H143), C140(H140), C141(H141),
 C156(H156), C152(H152), C153(H153), C155(H155), C158(H158), C163(H163),
 C162(H162), C161(H161), C160(H160), C215(H215), C216(H216), C212(H212),
 C213(H213), C218(H218), C223(H223), C222(H222), C221(H221), C220(H220),
 C235(H235), C236(H236), C232(H232), C233(H233), C238(H238), C243(H243),
 C240(H240), C241(H241), C242(H242), C255(H255), C256(H256), C252(H252),
 C253(H253), C258(H258), C263(H263), C262(H262), C261(H261), C260(H260)
5.c Fitted hexagon refined as free rotating group:
 C116(C111,C112,C113,C114,C115), C123(N124,C119,C120,C121,C122), C136(C131,
 C132,C133,C134,C135), C142(C143,N144,C139,C140,C141), C156(C151,C152,C153,C154,
 C155), C163(C162,C161,C160,C159,N164), C215(C216,C211,C212,C213,C214),
 C223(C222,C221,C220,C219,N224), C234(C235,C236,C231,C232,C233), C243(N244,C239,
 C240,C241,C242), C255(C256,C251,C252,C253,C254), C263(C262,C261,C260,C259,N264)
;
_shelx_res_checksum              94328
_shelx_fab_checksum              97747
_olex2_submission_special_instructions 'No special instructions were received'