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_7710214
_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         'C92 H92 N4 O8 Rh4, 4(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C96 H98 F24 N6 O8 P4 Rh4'
_chemical_formula_weight         2455.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.277(7)
_cell_length_b                   22.228(6)
_cell_length_c                   41.74(3)
_cell_measurement_reflns_used    9774
_cell_measurement_temperature    192.0
_cell_measurement_theta_max      24.75
_cell_measurement_theta_min      2.32
_cell_volume                     22524(18)
_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  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      192.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0750
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            145730
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.685
_diffrn_reflns_theta_min         2.239
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0860 before and 0.0576 after correction.
The Ratio of minimum to maximum transmission is 0.8516.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             9888
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.009
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1301
_refine_ls_number_reflns         21326
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0596
_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^)+(0.1014P)^2^+14.6243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13197
_reflns_number_total             21326
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01094a2.cif
_cod_data_source_block           C96H98F24N6O8P4Rh4
_cod_original_cell_volume        22522(18)
_cod_database_code               7710214
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.869
_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.a Aromatic/amide H refined with riding coordinates:
 C00P(H00P), C00Q(H00Q), C00R(H00R), C00V(H00V), C00X(H00X), C00Y(H00Y),
 C00Z(H00Z), C010(H010), C012(H012), C016(H016), C018(H018), C01B(H01B),
 C01C(H01C), C01D(H01D), C01G(H01G), C01P(H01P), C01Q(H01Q), C01R(H01R),
 C022(H022), C023(H023), C024(H024), C028(H028), C029(H029), C02B(H02B),
 C02F(H02F), C02G(H02G), C02I(H02I), C02P(H02P), C02Q(H02Q), C02R(H02R),
 C02T(H02T), C02X(H02X)
2.b Idealised Me refined as rotating group:
 C02Y(H02a,H02c,H02d), C035(H03a,H03b,H03c), C039(H03d,H03e,H03f), C03A(H03g,
 H03h,H03i), C03B(H03j,H03k,H03l), C03D(H03m,H03n,H03o), C03E(H03p,H03q,H03r),
 C03F(H03s,H03t,H03u), C03G(H03v,H03w,H03x), C03H(H03y,H,Ha), C03I(H03z,Hb,Hc),
 C03J(H03,Hd,He), C03M(H1,Hf,Hg), C03N(H2,Hh,Hi), C03O(H3,Hj,Hk), C03P(H4,Hl,
 Hm), C03Q(H5,Hn,Ho), C03R(H6,Hp,Hq), C03S(H7,Hr,Hs), C03V(H8,Ht,Hu), C03W(H10,
 Hv,Hw), C03X(H9,Hx,Hy)
;
_shelx_res_checksum              50866
_shelx_fab_checksum              41179
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'