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_7123950
_publ_section_title
;
 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 S4, 8(B F4)'
_chemical_formula_sum            'C144 H108 B8 Co4 F32 N24 O12 P4 S4'
_chemical_formula_weight         3548.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-09-12
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.900(5)
_cell_length_b                   24.860(5)
_cell_length_c                   38.800(8)
_cell_measurement_reflns_used    3896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      0.4
_cell_volume                     22089(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 0.836
_diffrn_measured_fraction_theta_max 0.876
_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  0.0556
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.836
_diffrn_reflns_Laue_measured_fraction_max 0.876
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            192192
_diffrn_reflns_point_group_measured_fraction_full 0.834
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.818
_diffrn_reflns_theta_min         0.973
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_description       plate
_exptl_crystal_F_000             7184
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1739
_refine_ls_number_reflns         32756
_refine_ls_number_restraints     2224
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.1411
_refine_ls_R_factor_gt           0.1009
_refine_ls_shift/su_max          0.002
_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          0.2807
_refine_ls_wR_factor_ref         0.3107
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.831
_reflns_Friedel_fraction_max     0.873
_reflns_number_gt                19966
_reflns_number_total             32756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05443j2.cif
_cod_data_source_block           '[1d]'
_cod_database_code               7123950
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.918
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53(3)
 0.47(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Rigid bond restraints
 F112, F113, F114, F115, B111
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 F122, F123, F124, F125, B121
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 F152, F153, F154, F155, B151
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 F132, F133, F134, F135, B131
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
F142 \\sim F143 \\sim F144 \\sim F145 \\sim B141: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
F112 \\sim F113 \\sim F114 \\sim F115 \\sim B111: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
F122 \\sim F123 \\sim F124 \\sim F125 \\sim B121: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
C223 \\sim N224 \\sim C219 \\sim C220 \\sim C221 \\sim C222: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
N144 \\sim C139 \\sim C140 \\sim C141 \\sim C142 \\sim C143: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
F182 \\sim F183 \\sim F184 \\sim F185 \\sim B181: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
F152 \\sim F153 \\sim F154 \\sim F155 \\sim B151: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
F132 \\sim F133 \\sim F134 \\sim F135 \\sim B131: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
F172 \\sim F173 \\sim F174 \\sim F175 \\sim B171: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(C141) \\sim Ueq: with sigma of 0.025 and sigma for terminal atoms of 0.05
5. Rigid body (RIGU) restrains
 C141, Co1, N117, N217, N317, N124, N224, N324, C114, C118, C214, C218, C314,
 C318, C119, C123, C223, C219, C323, C319, C115, C113, H118, C215, C213, H218,
 C313, C315, H318, C120, C122, H123, H223, C222, C220, C322, H323, C320, H115,
 C116, H113, C112, C216, H215, H213, C212, H313, C312, C316, H315, H120, C121,
 H122, C221, H222, H220, C321, H322, H320, C111, H116, H112, H216, C211, H212,
 H312, C311, H316, H121, H221, H321, O11, O21, O31, P1, P2, P3, S1, O12, O13,
 S2, O22, O23, S3, O32, O33, C131, C151, C231, C251, C331, C351, C132, C136,
 C152, C156, C232, C236, C252, C256, C336, C332, C352, C356, C133, H132, H136,
 C135, C153, H152, C155, H156, C233, H232, H236, C235, C253, H252, H256, C255,
 H336, C335, C333, H332, C353, H352, C355, H356, H133, C134, H135, C154, H153,
 H155, C234, H233, H235, H253, C254, H255, H335, C334, H333, C354, H353, H355,
 N137, N157, N237, N257, N337, N357, Co2, C138, Co3, C158, C238, Co4, C258,
 C338, C358, N344, N417, N144, N424, H138, C139, N437, N164, N244, N444, H158,
 C159, H238, C239, N457, N264, N364, N464, H258, C259, C339, H338, H358, C359,
 C343, C414, C418, C143, C419, C423, C140, C434, C438, C163, C243, C439, C443,
 C160, C240, C454, C458, C263, C363, C459, C463, C260, C340, C360, C342, H343,
 C415, C413, H418, H143, C142, C420, H423, C422, H140, C435, C433, H438, C162,
 H163, H243, C242, C440, C442, H443, H160, C161, C241, H240, C455, C453, H458,
 C262, H263, C362, H363, C460, H463, C462, H260, C261, H340, C341, H360, C361,
 H342, C416, H415, H413, C412, H142, C421, H420, H422, H141, C436, H435, H433,
 C432, H162, H242, C441, H440, H442, H161, H241, H455, C456, C452, H453, H262,
 H362, C461, H460, H462, H261, H341, H361, C411, H416, H412, H421, C431, H436,
 H432, H441, H456, C451, H452, H461, O41, O42, O43, P4, S4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F182, F183, F184, F185, B181
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F162, F163, F164, F165, B161, F172, F173, F174, F175, B171
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6.a Free rotating group:
 B141(F142,F143,F144,F145), B161(F162,F163,F164,F165), B111(F112,F113,F114,
 F115), B151(F152,F153,F154,F155), B171(F172,F173,F174,F175), B131(F132,F133,
 F134,F135), B181(F182,F183,F184,F185)
6.b Aromatic/amide H refined with riding coordinates:
 C340(H340), C341(H341), C342(H342), C343(H343), C115(H115), C113(H113),
 C112(H112), C116(H116), C118(H118), C120(H120), C121(H121), C122(H122),
 C123(H123), C133(H133), C132(H132), C136(H136), C135(H135), C138(H138),
 C141(H141), C140(H140), C143(H143), C142(H142), C155(H155), C153(H153),
 C152(H152), C156(H156), C158(H158), C162(H162), C163(H163), C160(H160),
 C161(H161), C216(H216), C215(H215), C213(H213), C212(H212), C218(H218),
 C223(H223), C220(H220), C221(H221), C222(H222), C233(H233), C232(H232),
 C236(H236), C235(H235), C238(H238), C241(H241), C240(H240), C243(H243),
 C242(H242), C253(H253), C252(H252), C256(H256), C255(H255), C258(H258),
 C262(H262), C263(H263), C260(H260), C261(H261), C313(H313), C312(H312),
 C316(H316), C315(H315), C318(H318), C321(H321), C322(H322), C323(H323),
 C320(H320), C336(H336), C335(H335), C333(H333), C332(H332), C338(H338),
 C355(H355), C353(H353), C352(H352), C356(H356), C358(H358), C362(H362),
 C363(H363), C360(H360), C361(H361), C416(H416), C415(H415), C413(H413),
 C412(H412), C418(H418), C421(H421), C420(H420), C423(H423), C422(H422),
 C436(H436), C435(H435), C433(H433), C432(H432), C438(H438), C442(H442),
 C441(H441), C440(H440), C443(H443), C455(H455), C456(H456), C452(H452),
 C453(H453), C458(H458), C461(H461), C460(H460), C463(H463), C462(H462)
6.c Fitted hexagon refined as free rotating group:
 N344(C339,C340,C341,C342,C343), C115(C114,C113,C112,C111,C116), C119(C120,
 C121,C122,C123,N124), C133(C132,C131,C136,C135,C134), C141(C140,C139,N144,C143,
 C142), C155(C154,C153,C152,C151,C156), C162(C163,N164,C159,C160,C161),
 C216(C215,C214,C213,C212,C211), C223(N224,C219,C220,C221,C222), C234(C233,C232,
 C231,C236,C235), C241(C240,C239,N244,C243,C242), C253(C252,C251,C256,C255,
 C254), C262(C263,N264,C259,C260,C261), C313(C312,C311,C316,C315,C314),
 C321(C322,C323,N324,C319,C320), C331(C336,C335,C334,C333,C332), C355(C354,C353,
 C352,C351,C356), C362(C363,N364,C359,C360,C361), C411(C416,C415,C414,C413,
 C412), C421(C420,C419,N424,C423,C422), C431(C436,C435,C434,C433,C432),
 C442(C441,C440,C439,N444,C443), C455(C456,C451,C452,C453,C454), C461(C460,C459,
 N464,C463,C462)
;
_shelx_res_checksum              68802
_shelx_fab_checksum              87214
_olex2_submission_special_instructions 'No special instructions were received'