Supramolecular-controlled regioselective photochemical [4+4] cycloaddition within Cp*Rh-based metallarectangles
Bai, Sha; Wang, Li-Feng; Wu, Zhen-Wei; Feng, Ting; Han, Ying-Feng; Dalton Transactions  (2022) –; doi:10.1039/D2DT01094A

data_7710212
_publ_section_title
;
 Supramolecular-controlled regioselective photochemical [4+4]
 cycloaddition within Cp*Rh-based metallarectangles
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01094A
_journal_year                    2022
_chemical_formula_moiety         'C84 H88 N8 O8 Rh4, 1.5(C2 F6 O6 S2)'
_chemical_formula_sum            'C87 H88 F9 N8 O17 Rh4 S3'
_chemical_formula_weight         2196.47
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-04-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2022-04-07 deposited with the CCDC.	2022-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.9440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.7296(12)
_cell_length_b                   19.6924(8)
_cell_length_c                   23.9910(8)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      25.21
_cell_measurement_theta_min      2.28
_cell_volume                     11603.0(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            37812
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.378
_diffrn_reflns_theta_min         2.325
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0638 before and 0.0451 after correction.
The Ratio of minimum to maximum transmission is 0.8845.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       block
_exptl_crystal_F_000             4444
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.472
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         10418
_refine_ls_number_restraints     278
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1206
_refine_ls_R_factor_gt           0.0887
_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^)+(0.1604P)^2^+61.1721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2470
_refine_ls_wR_factor_ref         0.2802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6944
_reflns_number_total             10418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01094a2.cif
_cod_data_source_block           C87H88F9N8O17Rh4S3
_cod_database_code               7710212
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.848
_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
 S1-C23
 1.83 with sigma of 0.02
 S0AA-C27
 1.7 with sigma of 0.02
 S0AA-O8
 1.39 with sigma of 0.01
 F9-C23 = F43-C23 = F15-C23
 1.39 with sigma of 0.01
 S1-O33 = S1-O9 = S1-O7
 1.43 with sigma of 0.01
 F0AA-F14 \\sim F0AA-F4 \\sim F14-F4
 with sigma of 0.05
 F0AA-C27 \\sim F14-C27 \\sim F4-C27
 with sigma of 0.05
 S0AA-F0AA \\sim S0AA-F14 \\sim S0AA-F4
 with sigma of 0.05
 O8-O6 \\sim O8-O16 \\sim O6-O16
 with sigma of 0.05
 S0AA-O8 \\sim S0AA-O6 \\sim S0AA-O16
 with sigma of 0.05
 C27-O8 \\sim C27-O6 \\sim C27-O16
 with sigma of 0.05
 F9-F15 \\sim F9-F43 \\sim F15-F43
 with sigma of 0.05
 F9-C23 \\sim F15-C23 \\sim F43-C23
 with sigma of 0.05
 O33-O7 \\sim O33-O9 \\sim O7-O9
 with sigma of 0.05
 C23-O33 \\sim C23-O7 \\sim C23-O9
 with sigma of 0.05
 S1-O33 \\sim S1-O7 \\sim S1-O9
 with sigma of 0.05
 S1-F9 \\sim S1-F15 \\sim S1-F43
 with sigma of 0.05
3. Rigid bond restraints
 C10, C01G, C2, C16, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C7, C16, C2, C01G, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F0AA, F4, F14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C27, F4, F14, F0AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S0AA, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S0AA, O16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C019, C01H, C01H, C013, S0AA, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F9, S1, O7, O9, C23, F15, F43
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O9, S1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S1, O33
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S1, C23, O7, O9, F9, F15, S0AA, O8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F0AA \\sim S0AA \\sim O8 \\sim O16 \\sim C27 \\sim O6 \\sim F4 \\sim F14:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
O9 \\sim S1 \\sim O7 \\sim C23 \\sim O33 \\sim F15 \\sim F9 \\sim F43: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
Uanis(C7) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C019) \\sim Ueq, Uanis(C016) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(F14) \\sim Ueq, Uanis(F0AA) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(C27)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C27) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(S1) \\sim Ueq, Uanis(S0AA) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O33) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F43)
\\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(S1) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
5. Others
 Fixed Sof: O7(0.5) O9(0.5) F15(0.5) O33(0.5) F9(0.5) F43(0.5)
6.a Ternary CH refined with riding coordinates:
 C00H(H00H), C00P(H00P)
6.b Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00G(H00G), C00I(H00I), C00O(H00O), C00Q(H00Q), C00S(H00S),
 C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Z(H00Z)
6.c Fitted pentagon refined as free rotating group:
 C016(C019,C01H,C013,C015)
6.d Idealised Me refined as rotating group:
 C00Y(H00A,H00B,H00C), C017(H01A,H01B,H01C), C01D(H01D,H01E,H01F), C01E(H01G,
 H01H,H01I), C01G(H01J,H01K,H01L), C01K(H01M,H01N,H01O), C2(H2A,H2B,H2C),
 C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              88713
_shelx_fab_checksum              41206
_olex2_submission_special_instructions 'No special instructions were received'