Highly selective synthesis and near-infrared photothermal conversion of metalla-Borromean ring and [2]catenane assemblies
Dang, Li-Long; Li, Ting-Ting; Zhang, Ting-Ting; Zhao, Ying; Chen, Tian; Gao, Xiang; Ma, Lufang; Jin, Guo-Xin; Chemical Science  (2022) –; doi:10.1039/D2SC00437B

data_1566756
_publ_section_title
;
 Highly selective synthesis and near-infrared photothermal conversion of
 metalla-Borromean ring and [2]catenane assemblies
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC00437B
_journal_year                    2022
_chemical_formula_moiety         'C116 H100 N4 O8 Rh4, 6(C F3 O3 S)'
_chemical_formula_sum            'C122 H100 F18 N4 O26 Rh4 S6'
_chemical_formula_weight         2984.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-02-27
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-02-28 deposited with the CCDC.	2022-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.251(4)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   23.670(2)
_cell_length_b                   36.843(3)
_cell_length_c                   25.731(2)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      46.87
_cell_measurement_theta_min      3.23
_cell_volume                     20768(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.1129
_diffrn_reflns_av_unetI/netI     0.1269
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            125192
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.639
_diffrn_reflns_theta_min         2.987
_diffrn_source_current           2.85
_diffrn_source_power             0.1992435
_diffrn_source_voltage           69.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.586
_exptl_absorpt_correction_T_max  0.7505
_exptl_absorpt_correction_T_min  0.4489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1309 before and 0.0925 after correction.
The Ratio of minimum to maximum transmission is 0.5981.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       block
_exptl_crystal_F_000             9036
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.036
_refine_diff_density_min         -1.648
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2086
_refine_ls_number_reflns         36699
_refine_ls_number_restraints     4485
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1800
_refine_ls_R_factor_gt           0.1207
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+130.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2638
_refine_ls_wR_factor_ref         0.2901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16896
_reflns_number_total             36699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00437b2.cif
_cod_data_source_block           ga_220226a_a
_cod_depositor_comments
;

2025-07-10
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C366 H300 F54 N12 O78 Rh12 S18'
_cod_original_formula_weight         8952.16
_cod_original_formula_moiety
'3(C116 H100 N4 O8 Rh4), 8(C F3 O3 S), 10[CF3SO3]'
_cod_original_formula_units_Z            2
_cod_database_code               1566756
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.534
_shelx_estimated_absorpt_t_min   0.480
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O23-O19
 2.41 with sigma of 0.02
 F5-F3
 2.12 with sigma of 0.02
 S4-O9 = S4-O2 = S4-O7 = S2-O11 = S2-O17 = S2-O21 = S3-O23 = S3-O5 = S3-O19
 1.43 with sigma of 0.02
 F10-F8
 2.12 with sigma of 0.02
 F10-C167 = F8-C167 = F12-C167 = F5-C11 = F3-C11 = F11-C11 = F9-C177 = F2-C177
 = F7-C177
 1.33 with sigma of 0.02
 F9-F7
 2.12 with sigma of 0.02
 O2-O7 = O7-O9
 2.41 with sigma of 0.02
 F10-F12 = F12-F8
 2.12 with sigma of 0.02
 O2-O9
 2.41 with sigma of 0.02
 F5-F11 = F11-F3
 2.12 with sigma of 0.02
 O11-O17 = O17-O21
 2.41 with sigma of 0.02
 F9-F2 = F2-F7
 2.12 with sigma of 0.02
 O11-O21
 2.41 with sigma of 0.02
 O23-O5 = O5-O19
 2.41 with sigma of 0.02
 F8-S4
 2.6 with sigma of 0.02
 O19-C177
 2.55 with sigma of 0.02
 F12-S4
 2.6 with sigma of 0.02
 F3-S2
 2.6 with sigma of 0.02
 F7-S3
 2.6 with sigma of 0.02
 O7-C167
 2.55 with sigma of 0.02
 O23-C177
 2.55 with sigma of 0.02
 O11-C11
 2.55 with sigma of 0.02
 F2-S3
 2.6 with sigma of 0.02
 O17-C11
 2.55 with sigma of 0.02
 F9-S3
 2.6 with sigma of 0.02
 O21-C11
 2.55 with sigma of 0.02
 F10-S4
 2.6 with sigma of 0.02
 O5-C177
 2.55 with sigma of 0.02
 F5-S2
 2.6 with sigma of 0.02
 O9-C167
 2.55 with sigma of 0.02
 F11-S2
 2.6 with sigma of 0.02
 O2-C167
 2.55 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(S3) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(O19) \\sim
Ueq, Uanis(F9) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C177) \\sim Ueq,
Uanis(O23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S2) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F5) \\sim
Ueq, Uanis(F11) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O11) \\sim Ueq,
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S3) = Uanis(S4)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C16(H16), C24(H24), C26(H26), C34(H34), C44(H44), C70(H70),
 C74(H74), C78(H78), C84(H84), C86(H86), C90(H90), C94(H94), C98(H98),
 C100(H100), C102(H102), C104(H104), C108(H108), C110(H110), C112(H112),
 C114(H114), C122(H122), C124(H124), C126(H126), C130(H130), C132(H132),
 C136(H136), C140(H140), C144(H144), C146(H146), C148(H148), C152(H152),
 C156(H156), C164(H164), C168(H168), C174(H174), C89(H89), C45(H45), C93(H93),
 C95(H95), C3(H3), C97(H97), C49(H49), C99(H99), C25(H25), C51(H51), C27(H27),
 C109(H109), C57(H57), C59(H59), C119(H119), C121(H121), C65(H65), C35(H35),
 C143(H143), C9(H9), C149(H149), C151(H151), C155(H155), C39(H39)
6.b Fitted pentagon refined as free rotating group:
 C125(C135,C169,C79,C162)
6.c Idealised Me refined as rotating group:
 C158(H15A,H15B,H15C), C53(H53A,H53B,H53C), C7(H7A,H7B,H7C), C123(H12A,H12B,
 H12C), C31(H31A,H31B,H31C), C63(H63A,H63B,H63C), C67(H67A,H67B,H67C),
 C139(H13A,H13B,H13C), C141(H14A,H14B,H14C), C71(H71A,H71B,H71C), C147(H14D,
 H14E,H14F), C37(H37A,H37B,H37C), C75(H75A,H75B,H75C), C19(H19A,H19B,H19C),
 C153(H15D,H15E,H15F), C77(H77A,H77B,H77C), C159(H15G,H15H,H15I), C5(H5A,H5B,
 H5C), C161(H16D,H16E,H16F), C81(H81A,H81B,H81C), C163(H16G,H16H,H16I),
 C41(H41A,H41B,H41C), C165(H16A,H16B,H16C), C83(H83A,H83B,H83C), C21(H21A,H21B,
 H21C), C171(H17A,H17B,H17C), C43(H43A,H43B,H43C), C173(H17D,H17E,H17F),
 C87(H87A,H87B,H87C), C175(H17G,H17H,H17I)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1389 electrons were 
found in a volume of 6341\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
5[CF3SO3] per Asymmetric Unit 
which account for 1460 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              63306
_shelx_hkl_checksum              37307
_shelx_fab_checksum              33605
_olex2_submission_special_instructions 'No special instructions were received'