Light-initiated reversible conversion of macrocyclic endoperoxides derived from half-sandwich rhodium-based metallarectangles.
Shan, Wei-Long; Gao, Wen-Xi; Lin, Yue-Jian; Jin, Guo-Xin; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2769–2777; doi:10.1039/c7dt03962j

data_7045374
_publ_section_title
;
 Light-initiated reversible conversion of macrocyclic endoperoxides
 derived from half-sandwich rhodium-based metallarectangles.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2769
_journal_page_last               2777
_journal_paper_doi               10.1039/c7dt03962j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C136 H148 F12 N12 O26 Rh4 S4'
_chemical_formula_weight         3134.54
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-09-20 deposited with the CCDC.
2018-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.052(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.637(3)
_cell_length_b                   14.6321(17)
_cell_length_c                   23.470(3)
_cell_measurement_reflns_used    7591
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.25
_cell_volume                     7316.4(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_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  0.0675
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49258
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.949
_diffrn_reflns_theta_min         0.956
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.250
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 solvents (three acetonitrile molecules) which could not be 
 restrained properly. Therefore, SQUEEZE algorithm was used 
 to omit them. 
;
_refine_diff_density_max         4.207
_refine_diff_density_min         -1.687
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         15657
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1230
_refine_ls_R_factor_gt           0.0799
_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^)+(0.1672P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2271
_refine_ls_wR_factor_ref         0.2558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9387
_reflns_number_total             15657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03962j2.cif
_cod_data_source_block           6-O2
_cod_depositor_comments
'Adding full bibliography for 7045371--7045376.cif.'
_cod_original_cell_volume        7316.4(14)
_cod_database_code               7045374
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.795
_shelx_estimated_absorpt_t_max   0.867
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              56854