Host-guest capability of a three-dimensional heterometallic macrocycle.
Fan, Qi-Jia; Lin, Yue-Jian; Hahn, F. Ekkehardt; Jin, Guo-Xin; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2240–2246; doi:10.1039/c7dt04453d

data_7045243
_publ_section_title
;
 Host-guest capability of a three-dimensional heterometallic macrocycle.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2240
_journal_page_last               2246
_journal_paper_doi               10.1039/c7dt04453d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'0.67(C128 H152 Cl4 Cu4 N4 O27.5 Rh4), 0.33(C130 H158 Cl4 Cu4 N4 O28 Rh4), 2.67(C F3 O3 S), C16 H10, 0.67(C4 H10 O), 0.67(C O)'
_chemical_formula_sum            'C154 H192 Cl4 Cu4 F12 N4 O45 Rh4 S4'
_chemical_formula_weight         3982.94
_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   geom
_audit_creation_date             2018-01-08
_audit_creation_method
; 
Olex2 1.2-beta 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_audit_update_record
;
2018-01-08 deposited with the CCDC.
2018-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                80.7437(17)
_cell_angle_beta                 85.6454(17)
_cell_angle_gamma                70.2326(17)
_cell_formula_units_Z            3
_cell_length_a                   18.9815(9)
_cell_length_b                   23.9885(11)
_cell_length_c                   34.8027(16)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      68.38
_cell_measurement_theta_min      2.82
_cell_volume                     14715.0(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0880
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            97360
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.999
_diffrn_reflns_theta_min         2.198
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.694
_exptl_absorpt_correction_T_max  0.1665
_exptl_absorpt_correction_T_min  0.0465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. 
wR2(int) was 0.1445 before and 0.0759 after correction. 
The Ratio of minimum to maximum transmission is 0.2793. 
The \l/2 correction factor is 0.00150. 
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       block
_exptl_crystal_F_000             6120
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.27
_platon_squeeze_details
;
 In asymmetric unit of this data, there were disordered
 anions and solvents (two triflate anions, three methanol
 and three water molecules) which could not be restrained
 properly. Therefore, SQUEEZE algorithm was used to omit
 them.
;
_refine_diff_density_max         2.579
_refine_diff_density_min         -4.999
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.445
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3207
_refine_ls_number_reflns         50550
_refine_ls_number_restraints     738
_refine_ls_restrained_S_all      1.456
_refine_ls_R_factor_all          0.1631
_refine_ls_R_factor_gt           0.1306
_refine_ls_shift/su_max          0.006
_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          0.3776
_refine_ls_wR_factor_ref         0.4110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32130
_reflns_number_total             50550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04453d2.cif
_cod_data_source_block           G1_1a
_cod_depositor_comments
'Adding full bibliography for 7045239--7045244.cif.'
_cod_database_code               7045243
_shelx_estimated_absorpt_t_max   0.364
_shelx_estimated_absorpt_t_min   0.306
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2. Shared sites 
{C57, C57'} 
{C76, C76'} 
3. Restrained distances 
 O46-O47 = O46-O48 = O47-O48 
 2.4 with sigma of 0.03 
 S2-O40 = S2-O41 = S2-O42 
 1.41 with sigma of 0.01 
 S4-O47 
 1.42 with sigma of 0.02 
 O55-C224 = O55-C225 = O60-C227 
 1.42 with sigma of 0.03 
 C202-C203 = C203-C204 
 1.4 with sigma of 0.02 
 F10-F11 = F10-F12 = F11-F12 
 2.1 with sigma of 0.03 
 C194-F4 = C195-F8 = C196-F10 = C196-F11 = C196-F12 
 1.35 with sigma of 0.02 
 S3-O43 = S3-O44 = S3-O45 = S4-O46 = S4-O47 = S4-O48 
 1.42 with sigma of 0.02 
 S4-C196 
 1.8 with sigma of 0.02 
 C175-C176 = C176-C177 
 1.4 with sigma of 0.02 
 C251-C252 = C251-C253 = C252-C253 
 2.5 with sigma of 0.03 
 C150-C251 = C150-C252 = C150-C253 
 1.52 with sigma of 0.02 
 C151-C152 = C151-C153 = C152-C153 
 2.5 with sigma of 0.03 
 C150-C151 = C150-C152 = C150-C153 
 1.52 with sigma of 0.02 
 C79-C80 = C79-C81 = C80-C81 = C79'-C80' = C79'-C81' = C80'-C81' 
 2.5 with sigma of 0.03 
 C78-C79 = C78-C80 = C78-C81 = C78'-C79' = C78'-C80' = C78'-C81' 
 1.52 with sigma of 0.02 
 C66-C68 = C85-C88 
 1.52 with sigma of 0.02 
 C60-C61 = C60-C62 = C61-C62 = C60'-C61' = C60'-C62' = C61'-C62' 
 2.5 with sigma of 0.03 
 C59-C60 = C59-C61 = C59-C62 = C59'-C60' = C59'-C61' = C59'-C62' 
 1.52 with sigma of 0.02 
 C48-C49 = C48-C50 = C49-C50 = C48'-C49' = C48'-C50' = C49'-C50' 
 2.5 with sigma of 0.03 
 C47-C48 = C47-C49 = C47-C50 = C47'-C48' = C47'-C49' = C47'-C50' 
 1.52 with sigma of 0.02 
 C41-C42 = C41-C43 = C42-C43 = C41'-C42' = C41'-C43' = C42'-C43' 
 2.5 with sigma of 0.03 
 C40-C41 = C40-C42 = C40-C43 = C40'-C41' = C40'-C42' = C40'-C43' 
 1.52 with sigma of 0.02 
 C27-C29 = C27-C31 = C39-C42' = C46-C48' = C58-C60 = C58'-C60' 
 2.5 with sigma of 0.03 
 C29-C30 = C29-C31 = C30-C31 = C29'-C30' = C29'-C31' = C30'-C31' 
 2.5 with sigma of 0.03 
 C28-C29 = C28-C30 = C28-C31 = C28-C29' = C28-C30' = C28-C31' 
 1.52 with sigma of 0.02 
 C122-C127 = C175-C180 
 1.5 with sigma of 0.02 
 C77-C78 = C77'-C78' 
 1.5 with sigma of 0.02 
 C27-C28 = C39-C40 = C46-C47' = C58-C59 = C58'-C59' 
 1.5 with sigma of 0.02 
 C223-C224 = C225-C226 
 1.52 with sigma of 0.03 
4. Uiso/Uaniso restraints and constraints 
C196 \\sim F10 \\sim F11 \\sim F12: within 2A with sigma of 0.02 and sigma for 
terminal atoms of 0.05 
Cu3' \\sim O58: within 2A with sigma of 0.02 and sigma for terminal atoms of 
0.05 
Uanis(Cu1) \\sim Ueq, Uanis(Cu2) \\sim Ueq, Uanis(Cu3) \\sim Ueq, Uanis(Cu4) 
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(O9) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O16) 
\\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O38) \\sim Ueq, 
Uanis(O43) \\sim Ueq, Uanis(O44) \\sim Ueq, Uanis(O45) \\sim Ueq, Uanis(O47) 
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(F3) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim 
Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq: with 
sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C20) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) 
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C29') \\sim Ueq, 
Uanis(C30') \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C78') \\sim Ueq, Uanis(C80') 
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) 
\\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C41') \\sim Ueq, Uanis(C42') \\sim Ueq, 
Uanis(C43') \\sim Ueq, Uanis(C47') \\sim Ueq, Uanis(C48') \\sim Ueq, 
Uanis(C49') \\sim Ueq, Uanis(C50') \\sim Ueq: with sigma of 0.02 and sigma for 
terminal atoms of 0.04 
Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60) 
\\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(O17) \\sim Ueq, 
Uanis(C57') \\sim Ueq, Uanis(C58') \\sim Ueq, Uanis(C59') \\sim Ueq, 
Uanis(C60') \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C61') \\sim Ueq, Uanis(C62') \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) 
\\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C76) \\sim Ueq, 
Uanis(C77) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C80) \\sim Ueq: with sigma of 
0.02 and sigma for terminal atoms of 0.04 
Uanis(C87) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C111) \\sim Ueq, Uanis(C126) 
\\sim Ueq, Uanis(C127) \\sim Ueq, Uanis(C128) \\sim Ueq, Uanis(C145) \\sim Ueq, 
Uanis(C146) \\sim Ueq, Uanis(C153) \\sim Ueq: with sigma of 0.02 and sigma for 
terminal atoms of 0.04 
Uanis(C251) \\sim Ueq, Uanis(C252) \\sim Ueq, Uanis(C253) \\sim Ueq, 
Uanis(C171) \\sim Ueq, Uanis(C172) \\sim Ueq, Uanis(C176) \\sim Ueq, 
Uanis(C179) \\sim Ueq, Uanis(C180) \\sim Ueq, Uanis(C181) \\sim Ueq: with sigma 
of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C195) \\sim Ueq, Uanis(C202) \\sim Ueq, Uanis(C203) \\sim Ueq, 
Uanis(C204) \\sim Ueq, Uanis(C205) \\sim Ueq, Uanis(C207) \\sim Ueq, 
Uanis(C208) \\sim Ueq, Uanis(C209) \\sim Ueq, Uanis(C225) \\sim Ueq, 
Uanis(C226) \\sim Ueq, Uanis(O57) \\sim Ueq: with sigma of 0.02 and sigma for 
terminal atoms of 0.04 
Uanis(C182) \\sim Ueq, Uanis(O58) \\sim Ueq: with sigma of 0.01 and sigma for 
terminal atoms of 0.02 
Uanis(C31') \\sim Ueq, Uanis(C79') \\sim Ueq: with sigma of 0.005 and sigma for 
terminal atoms of 0.01 
Uanis(Cu1) = Uanis(Cu1') 
Uanis(Cu2) = Uanis(Cu2') 
Uanis(Cu3) = Uanis(Cu3') 
Uanis(Cu4) = Uanis(Cu4') 
Uanis(C57) = Uanis(C57') 
Uanis(C76) = Uanis(C76') 
Uanis(C78) = Uanis(C78') 
Uanis(C81) = Uanis(C81') 
5. Others 
 Sof(Cu1')=Sof(C40')=Sof(C41')=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42')= 
 Sof(H42D)=Sof(H42E)=Sof(H42F)=Sof(C43')=Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(1) 
 Sof(Cu1)=Sof(C40)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)= 
 Sof(H42B)=Sof(H42C)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(1) 
 Sof(Cu2')=Sof(C29')=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30')=Sof(H30D)= 
 Sof(H30E)=Sof(H30F)=Sof(C31')=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C47')= 
 Sof(C48')=Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(C49')=Sof(H49D)=Sof(H49E)= 
 Sof(H49F)=Sof(C50')=Sof(H50D)=Sof(H50E)=Sof(H50F)=1-FVAR(2) 
 Sof(Cu2)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)= 
 Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C47)=Sof(C48)=Sof(H48A)= 
 Sof(H48B)=Sof(H48C)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C50)=Sof(H50A)= 
 Sof(H50B)=Sof(H50C)=FVAR(2) 
 Sof(Cu3')=Sof(C57')=Sof(H57')=Sof(C58')=Sof(C59')=Sof(C60')=Sof(H60D)= 
 Sof(H60E)=Sof(H60F)=Sof(C61')=Sof(H61D)=Sof(H61E)=Sof(H61F)=Sof(C62')= 
 Sof(H62D)=Sof(H62E)=Sof(H62F)=Sof(O17')=Sof(C76')=Sof(H76')=Sof(C77')= 
 Sof(C78')=Sof(C79')=Sof(H79D)=Sof(H79E)=Sof(H79F)=Sof(C80')=Sof(H80D)= 
 Sof(H80E)=Sof(H80F)=Sof(C81')=Sof(H81D)=Sof(H81E)=Sof(H81F)=Sof(O21')=1-FVAR(3) 
 Sof(Cu3)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(C59)=Sof(C60)=Sof(H60A)=Sof(H60B)= 
 Sof(H60C)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(C62)=Sof(H62A)=Sof(H62B)= 
 Sof(H62C)=Sof(O17)=Sof(C76)=Sof(H76)=Sof(C77)=Sof(C78)=Sof(C79)=Sof(H79A)= 
 Sof(H79B)=Sof(H79C)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=Sof(C81)=Sof(H81A)= 
 Sof(H81B)=Sof(H81C)=Sof(O21)=FVAR(3) 
 Sof(Cu4')=1-FVAR(4) 
 Sof(Cu4)=FVAR(4) 
 Sof(C251)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C252)=Sof(H25D)=Sof(H25E)= 
 Sof(H25F)=Sof(C253)=Sof(H25G)=Sof(H25H)=Sof(H25I)=1-FVAR(5) 
 Sof(C151)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C152)=Sof(H15D)=Sof(H15E)= 
 Sof(H15F)=Sof(C153)=Sof(H15G)=Sof(H15H)=Sof(H15I)=FVAR(5) 
 Fixed Sof: O57(0.5) 
6.a Secondary CH2 refined with riding coordinates: 
 C224(H22J,H22K), C225(H22L,H22M) 
6.b Me refined with riding coordinates: 
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C29'(H29D,H29E,H29F), C30'(H30D, 
 H30E,H30F), C79(H79A,H79B,H79C), C81(H81A,H81B,H81C), C81'(H81D,H81E,H81F), 
 C253(H25G,H25H,H25I) 
6.c Aromatic/amide H refined with riding coordinates: 
 C13(H13), C15(H15), C17(H17), C19(H19), C26(H26), C32(H32), C34(H34), 
 C36(H36), C38(H38), C45(H45), C51(H51), C53(H53), C55(H55), C57(H57), 
 C57'(H57'), C64(H64), C70(H70), C72(H72), C74(H74), C76(H76), C76'(H76'), 
 C83(H83), C135(H135), C137(H137), C139(H139), C141(H141), C148(H148), 
 C154(H154), C156(H156), C158(H158), C160(H160), C167(H167), C200(H200), 
 C201(H201), C203(H203), C204(H204), C205(H205), C207(H207), C208(H208), 
 C210(H210), C211(H211), C212(H212), C215(H215), C216(H216), C218(H218), 
 C219(H219), C220(H220) 
6.d Idealised Me refined as rotating group: 
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C31(H31A,H31B, 
 H31C), C31'(H31D,H31E,H31F), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), 
 C43(H43A,H43B,H43C), C41'(H41D,H41E,H41F), C42'(H42D,H42E,H42F), C43'(H43D, 
 H43E,H43F), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), 
 C48'(H48D,H48E,H48F), C49'(H49D,H49E,H49F), C50'(H50D,H50E,H50F), C60(H60A, 
 H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C60'(H60D,H60E,H60F), 
 C61'(H61D,H61E,H61F), C62'(H62D,H62E,H62F), C67(H67A,H67B,H67C), C68(H68A,H68B, 
 H68C), C69(H69A,H69B,H69C), C80(H80A,H80B,H80C), C79'(H79D,H79E,H79F), 
 C80'(H80D,H80E,H80F), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C88(H88A,H88B, 
 H88C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C), C97(H97A, 
 H97B,H97C), C98(H98A,H98B,H98C), C104(H10A,H10B,H10C), C105(H10D,H10E,H10F), 
 C106(H10G,H10H,H10I), C107(H10J,H10K,H10L), C108(H10M,H10N,H10O), C114(H11A, 
 H11B,H11C), C115(H11D,H11E,H11F), C116(H11G,H11H,H11I), C117(H11J,H11K,H11L), 
 C118(H11M,H11N,H11O), C124(H12A,H12B,H12C), C125(H12D,H12E,H12F), C126(H12G, 
 H12H,H12I), C127(H12J,H12K,H12L), C128(H12M,H12N,H12O), C144(H14A,H14B,H14C), 
 C145(H14D,H14E,H14F), C146(H14G,H14H,H14I), C151(H15A,H15B,H15C), C152(H15D, 
 H15E,H15F), C153(H15G,H15H,H15I), C251(H25A,H25B,H25C), C252(H25D,H25E,H25F), 
 C163(H16A,H16B,H16C), C164(H16D,H16E,H16F), C165(H16G,H16H,H16I), C170(H17A, 
 H17B,H17C), C171(H17D,H17E,H17F), C172(H17G,H17H,H17I), C178(H17J,H17K,H17L), 
 C179(H17M,H17N,H17O), C180(H18A,H18B,H18C), C181(H18D,H18E,H18F), C182(H18G, 
 H18H,H18I), C188(H18J,H18K,H18L), C189(H18M,H18N,H18O), C190(H19A,H19B,H19C), 
 C191(H19D,H19E,H19F), C192(H19G,H19H,H19I), C223(H22G,H22H,H22I), C226(H22N, 
 H22O,H22P), C227(H22D,H22E,H22F) 
;
_shelx_res_checksum              36676
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'