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_7710213
_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
'2(C42 H44 N4 O4 Rh2), 4(C F3 O3 S), 2(C3 H7 N O)'
_chemical_formula_sum            'C94 H102 F12 N10 O22 Rh4 S4'
_chemical_formula_weight         2491.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/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                 100.3480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.3105(9)
_cell_length_b                   22.2812(8)
_cell_length_c                   22.7128(7)
_cell_measurement_reflns_used    9339
_cell_measurement_temperature    199.99
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.29
_cell_volume                     11604.8(7)
_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      199.99
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0703
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            103665
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.366
_diffrn_reflns_theta_min         2.161
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  0.2590
_exptl_absorpt_correction_T_min  0.2224
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1103 before and 0.0547 after correction.
The Ratio of minimum to maximum transmission is 0.8587.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       block
_exptl_crystal_F_000             5056
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.048
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1356
_refine_ls_number_reflns         21199
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0806P)^2^+20.3665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14057
_reflns_number_total             21199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01094a2.cif
_cod_data_source_block           C94H102F12N10O22Rh4S4
_cod_database_code               7710213
_shelx_shelxl_version_number     2018/3
_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
 N9-C90 = N9-C89
 1.36 with sigma of 0.01
 C18-C13
 1.54 with sigma of 0.02
 S4-C88 = S5-C88
 1.8 with sigma of 0.02
 S4-O20 = S4-O19 = S5-O19 = S4-O18 = S5-O18 = S5-O21
 1.4 with sigma of 0.02
 F10-C88 \\sim F11-C88 \\sim F12-C88
 with sigma of 0.05
3. Rigid bond restraints
 F3, C86, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C1, C2, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 F10, C88
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C89 \\sim N9 \\sim C90: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O23 \\sim C94 \\sim N10 \\sim C93 \\sim C92: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C85 \\sim F9 \\sim F7 \\sim F8: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C88 \\sim F10 \\sim F12 \\sim F11: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
S5 \\sim S4 \\sim O18 \\sim O20 \\sim O19 \\sim O21: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C89) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O23) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C92)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F7) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F8) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C88) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O21) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: S4(0.6) S5(0.4) O20(0.6) O21(0.4)
6.a Me refined with riding coordinates:
 C18(H18A,H18B,H18C)
6.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C65(H65), C32(H32), C66(H66), C40(H40), C81(H81), C69(H69),
 C37(H37), C72(H72), C70(H70), C67(H67), C74(H74), C79(H79), C34(H34), C42(H42),
  C39(H39), C23(H23), C41(H41), C28(H28), C82(H82), C84(H84), C35(H35),
 C83(H83), C27(H27), C25(H25), C24(H24), C77(H77), C76(H76), C91(H91), C94(H94)
6.c Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C62(H62A,H62B,H62C), C61(H61A,H61B,H61C), C63(H63A,H63B,
 H63C), C21(H21A,H21B,H21C), C60(H60A,H60B,H60C), C22(H22A,H22B,H22C), C54(H54A,
 H54B,H54C), C20(H20A,H20B,H20C), C53(H53A,H53B,H53C), C19(H19A,H19B,H19C),
 C51(H51A,H51B,H51C), C50(H50A,H50B,H50C), C90(H90A,H90B,H90C), C52(H52A,H52B,
 H52C), C10(H10A,H10B,H10C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C7(H7A,H7B,H7C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C89(H89A,H89B,H89C)
;
_shelx_res_checksum              61987
_shelx_fab_checksum              86225
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'